Month: May 2021

Synthetic Route of 4254-29-9, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 4254-29-9, name is 2,3-Dihydro-1H-inden-2-ol. A new synthetic method of this compound is introduced below.

General procedure: General Procedure C A flame-dried flask with Teflon stir bar was charged with triphenylphosphine (1.2 equiv.) and I2(1.2 equiv.) in CH2Cl2, the mixture was stirred for 10 min at room temperature. Imidazole (1.2equiv.) was added to the resulting mixture. After 10 min of stirring, the corresponding alcohol(1.0 equiv.) was added and the reaction was stirred for additional 5 h at room temperature andwas checked by TLC until completion. The reaction mixture was quenched with Sat. Na2SO3.The mixture was transferred to a separatory funnel using CH2Cl2 and brine to aid the transferand separation. The aqueous and organic layers were separated and the aqueous layer wasextracted by CH2Cl2 (3x). The combined organic layers were washed with brine and dried overNa2SO4, filtered, and concentrated in vacuum. The crude reaction mixture was purified by flashchromatograph on silica gel and evaporated to give the alkyl iodide compound.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,4254-29-9, its application will become more common.

Reference:
Article; Bai, Songlin; Gao, Yadong; Jiang, Chao; Liu, Xiaolei; Qi, Xiangbing; Wang, Jing; Wu, Qingcui; Yang, Chao; Chem; vol. 6; 3; (2020); p. 675 – 688;,
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Synthetic Route of 1113-21-9, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 1113-21-9, name is 3,7,11,15-Tetramethylhexadeca-1,6,10,14-tetraen-3-ol. This compound has unique chemical properties. The synthetic route is as follows.

Example 5: 5E,9E,13E-Geranylgeranyl Acetone Synthesis[0141] Alternative synthesis of 5-trans Isomer: 5E,9E,13E-Geranylgeranyl acetone 1: The alternative synthesis of 5E,9E,13E-geranylgeranyl acetone 1 can be achieved as shown in the scheme-5.Scheme 5:[0142] The 5E, 9E, 13E-geranyl geranyl acetone (1) can be prepared by reacting 6E-10E- geranyl linalool (23) with diketene (24) catalyzed by DMAP in ethyl ether to give the ester 25. The ester 25 in the Carroll rearrangement using Al(OiPr)3 at elevated temperature can afford the desired 5E, 9E, 13E-geranyl geranyl acetone (1). In another approach, the GGA (1) can be prepared by treating geranyl linalool (23) with the Meldrum’s acid 26 in the Carroll rearrangement using Al(OiPr)3 at 160 C. Similarly, the use of tert-butyl acetoacetate (27) with geranyl linalool (23) in the Carroll rearrangement can also give the desired 5E, 9E, 13E-geranyl geranyl acetone (1).

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 1113-21-9, 3,7,11,15-Tetramethylhexadeca-1,6,10,14-tetraen-3-ol.

Reference:
Patent; COYOTE PHARMACEUTICALS, INC.; BARRES, Ben A.; NAKAYAMA, Naoki; SERIZAWA, Hiroaki; ARGADE, Ankush B.; WO2012/31028; (2012); A2;,
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With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.39590-81-3, name is 1,1-Bis(Hydroxymethyl)cyclopropane, molecular formula is C5H10O2, molecular weight is 102.13, as common compound, the synthetic route is as follows.Formula: C5H10O2

a) [1-[5-Methyl-3-(quinolinyl-8-sulfonyloxy)phenoxy]methyl]-cyclopropylmethanol To 250 mg (0.75 mmol) of 5-methyl-3-(quinolinyl-8-sulfonyloxy)phenol, as prepared in step a of example 15, 170 mg (1.7 mmol) of 1,1-di(hydroxymethyl)cyclopropane (as prepared in US Patent 5472964), and 370 muL (1.49 mmol) of tri-n-butylphosphine in 5 mL of anhydrous tetrahydrofuran was added 378 mg (1.5 mmol) of 1,1′-(azodicarbonyl)dipiperidine. The reaction mixture was stirred at ambient temperature for 2 days. The reaction mixture was diluted with diethyl ether, filtered, and the filtrate concentrated. The residue was purified by flash chromatography (dichloromethane / ethyl acetate (2: 1 to 1: 1)) to give the title compound as a gum (177 mg. 59%). 1H-NMR (300 MHz, CDCl3) delta 9.27 (dd, 1 H, J = 2, 4 Hz), 8.42 (dd, 1 H, J = 1.5,7.5 Hz), 8.30 (dd, 1 H, J = 2, 8 Hz), 7.06 – 7.65 (m, 2 H), 6.56 (s, 1 H), 6.44 – 6.47 (m, 2 H), 3.73 (s, 2 H), 3.56 (d, 2 H, J = 5.5 Hz), 2.17 (s, 3 H), 1.79 (t, 1 H, J = 5.5 Hz), 0.53 – 0.62 (m, 4 H). Mass spectrum (MALDI-TOF, alpha-cyano-4-hydroxycinnamic acid matrix) calcd. for C21H21NO5S: 400.1 (M +H). Found: 399.8.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,39590-81-3, 1,1-Bis(Hydroxymethyl)cyclopropane, and friends who are interested can also refer to it.

Reference:
Patent; Ortho-McNeil Pharmaceutical, Inc.; EP906091; (2006); B1;,
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The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 14426-20-1, name is 2-(Diethylamino)ethanol hydrochloride. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 14426-20-1

General procedure: Chenodeoxycholic acid (2.0 g, 5.1 mmol), DMAP (0.92 g, 7.6 mmol) and diethylaminoethanol hydrochloride (1.17 g, 7.6 mmol) were mixed and dissolved in dichloromethane (15 mL). ), EDCI (1.46 g, 7.6 mmol) was added in portions. After stirring at room temperature for 3 hours, water and dichloromethane were added and extracted three times. The organic phase was washed twice with saturated ammonium chloride and washed with saturated brine.Dry Na2SO4, concentrate by filtration,After column chromatography, chenodeoxycholic acid 2-(diethylamino)ethyl ester (2.99 g, 80%) was obtained.2-(Diethylamino)ethyl chenodeoxycholate (2.0 g, 4.1 mmol) was dissolved in 10 mL of glacial acetic acid, heated to 50 C for 2 hours, and glacial acetic acid was concentrated to obtain chenodeoxycholic acid 2 -(Diethylamino)ethyl acetate (2.24 g, 100%).

With the rapid development of chemical substances, we look forward to future research findings about 14426-20-1.

Reference:
Patent; Ningbo Bai Naxi Pharmaceutical Co., Ltd.; Li Xiaochuan; (20 pag.)CN108218945; (2018); A;,
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Related Products of 627-27-0, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 627-27-0, name is But-3-en-1-ol, molecular formula is C4H8O, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

But-3-en-1-yl methanesulfonate 8 was prepared from 3-buten-1-ol using the protocol described byD. Pei et al.:2 methanesulfonyl chloride (1.10 equiv, 110 mmol, 8.51 mL) was added dropwise to asolution of 3-buten-1-ol (1.00 equiv, 100 mmol, 7.21 g) and triethylamine (1.10 equiv, 110 mmol,15.3 mL) in CH2Cl2 (0.20 L) at 0 C. The mixture became cloudy. After 5 min of stirring, the coldbath was removed and stirring was continued for 1 h. The reaction mixture was then washed withsaturated NaHCO3 aqueous solution (0.10 L) and H2O (0.10 L). The organic layer was dried overMgSO4, filtered and concentrated to afford mesylate 8 (14.3 g, 95.2 mmol, 95%) as a colourless oilthat was used as such, without purification.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 627-27-0, But-3-en-1-ol.

Reference:
Article; Wolan, Andrzej; Kowalska-Six, Justyna A.; Rajerison, Holisoa; Cesario, Michele; Cordier, Marie; Six, Yvan; Tetrahedron; vol. 74; 38; (2018); p. 5248 – 5257;,
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Related Products of 52273-77-5, Adding some certain compound to certain chemical reactions, such as: 52273-77-5, name is 2-(3-Aminophenyl)ethanol,molecular formula is C8H11NO, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 52273-77-5.

(28B) Methyl trans-4-{[3-(2-hydroxyethyl)phenyl]amino}cyclohexanecarboxylate [0325] 2-(3-Aminophenyl)ethanol (4.45 g, 32.4 mmol) produced in (28A), ethyl 4-cyclohexanonecarboxylate (5.52 g, 32.4 mmol), and acetic acid (18.5 mL, 324 mmol) were dissolved in tetrahydrofuran (100 mL), and sodium triacetoxy borohydride (13.8 g, 64.9 mmol) was added thereto, and then, the resulting mixture was stirred at room temperature for 4 hours. To the reaction solution, water was added, and the organic matter was extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and then dried over anhydrous magnesium sulfate and filtered. Then, the solvent was distilled off under reduced pressure, whereby a crude product was obtained. The obtained crude product was purified by silica gel column chromatography (hexane:ethyl acetate = 70:30 to 45:55 (v/v)), whereby the target compound was obtained as a colorless oil (1.93 g, yield: 19%). 1H NMR(CDCl3, 400MHz): delta1.09-1.21(2H, m), 1.26(3H, t, J=7.2Hz), 1.51-1.65(2H, m), 2.01-2.10(2H, m), 2.16-2.24(2H, m), 2.29(1H, tt, J=3.6, 12.1Hz), 2.78(2H, t, J=6.5Hz), 3.25(1H, tt, J=3.6, 11.2Hz), 3.40-3.59(1H, brs), 3.84(2H, q, J=6.0Hz), 4.14(2H, q, J=7.2Hz), 6.41-6.49(2H, m), 6.55(1H, d, J=7.4Hz), 7.11(1H, t, J=7.6Hz).

According to the analysis of related databases, 52273-77-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Daiichi Sankyo Company, Limited; TODA, Narihiro; TAKANO, Rieko; SHIDA, Takeshi; KATAGIRI, Takahiro; IWAMOTO, Mitsuhiro; ASHIDA, Shinji; YAMAZAKI, Mami; EP2623492; (2013); A1;,
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The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 616-29-5, name is 1,3-Diaminopropan-2-ol. This compound has unique chemical properties. The synthetic route is as follows. Application In Synthesis of 1,3-Diaminopropan-2-ol

To a solution of 3-1 (3.00 g, 33.3 mmol) in dichloromethane (300 mL) was added triethylamine (5.10 mL, 36.6 mmol), 4-dimethylaminopyridine (DMAP, 40.7 mg, 0.333 mmol), and tert-butyldiphenylsilyl chloride (TBDPSCI, 9.13 mL, 35.0 mmol), and the mixture was stirred at room temperature for 5 hours. The solvent was removed by concentration in vacuo and chromatographed by flash chromatography on silica gel (chloroform/methanol = 5: 1) to give 3-2 (8.28 g, 76%). 1H MR (400 MHz, CDC13): delta 1.08 (s, 9H), 2.70-2.79 (m, 4H), 3.60-3.63 (m, 1H), 7.36-7.45 (m, 6H), 7.67-7.70 (m, 4H). MS (CI+) m/z: 329 (MH+).

With the rapid development of chemical substances, we look forward to future research findings about 616-29-5.

Reference:
Patent; MERCK SHARP & DOHME CORP.; INTERVET INTERNATIONAL B.V.; KYORIN PHARMACEUTICAL CO. LTD.; SINGH, Sheo B.; WARRASS, Ralf; ULLRICH, Joachim; KAWASHIMA, Mikako; FUKUDA, Yasumichi; TAKANO, Hisashi; (92 pag.)WO2016/123146; (2016); A1;,
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As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 112-47-0, name is 1,10-Decanediol, molecular formula is C10H22O2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. Recommanded Product: 112-47-0

EXAMPLE 3 10-Bromo-1-decanol A solution of 1,10-dihydroxydecane (80 g) in 47% hydrobromic acid (650 ml) was stirred at 80C whilst being continuously extracted with petroleum ether (boiling range 80-100), for 24 hours. The organic extracts were neutralised with solid potassium carbonate, filtered, and the filtrates evaporated to dryness. The resultant dark oil was fractionally distilled (Vigreaux apparatus) to give a colourless oil, boiling point 102-104 (0.01 mm Hg). Part of this oil (52 g) was purified by preparative HPLC (silica; eluents:diethyl ether/hexane 1:1) to remove a significant 1,10-dibromodecane impurity, finally yielding the title compound as a colourless oil.

With the rapid development of chemical substances, we look forward to future research findings about 112-47-0.

Reference:
Patent; Lilly Industries Limited; EP190042; (1991); B1;,
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Reference of 10488-69-4 ,Some common heterocyclic compound, 10488-69-4, molecular formula is C6H11ClO3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.

Example 14: Preparation of Ethyl (R)-4-CYANO-3-HYDROXYYRATE FROM ETHYL (S)-4-CHLORO-3- hydroxybutyrate To a 250 mL vessel connected to an automatic titrater by a pH electrode and a feeding tube for addition of base (7.5 M NaOH) was charged water (83.5 mL) and 0.7 g of halohydrin dehalogenase SEQ ID NO: 24. The mixture was stirred for 30 minutes. The titrater was activated and set to maintain pH 7. Then, 25percent aqueous HCN (9.26 ml, 8.6 g) was charged over 20 minute to make A 2.3percent HCN solution. The mixture was heated at 40 °C for 10 minutes, then ethyl (S) -4-chloro-3-hydroxybutyrate (5 g) was charged over 1 hour. The automatic titrater maintained the pH at 7 by the addition of 2M NaOH. After 20 hrs, GC analysis of a butyl acetate extract of a reaction sample showed the conversion of the ethyl (S)-4-CHLORO-3-HYDROXYBUTYRATE to ethyl (R)-4-CYANO-3-HYDROXYBUTYRATE was 95percent.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,10488-69-4, its application will become more common.

Reference:
Patent; CODEXIS, INC.; WO2005/18579; (2005); A2;,
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As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 2867-59-6, name is 3-Aminobutan-1-ol, molecular formula is C4H11NO, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. Quality Control of 3-Aminobutan-1-ol

75 g of D-malic acid (0.56 mol) in 250 ml of anhydrous ethanol, stirred at room temperature, the system was dissolved, then added dropwiseA 50 g mixture of 3-amino-1-butanol (0.56 mol) in racemic mixture was added dropwise and warmed to 30-40C. The system was dissolved and 0.5 g of (S)-3-amino-1-butanol was added. D Malate salt as a seed crystal, and stirring during heat preservation, the solid precipitated after half an hour, continue to stir for 2 to 3 hours, slowly to room temperature, and continue to cool to 5 to 10 C for half an hour, suction filtration, to obtain an optical purity of 90.8 %ee.The D-malate salt of (S)-3-amino-1-butanol.The resulting (S)-3-amino-1-butanol D-malate with an optical purity of 90.8% ee was suspended in 200 ml of anhydrous ethanol, warmed to reflux, and the system was dissolved, slowly cooled, and the cooling process was solid. Gradually precipitated, cooled to room temperature, stirred for 1~2 hours, continued cooling to 5~10C, and kept stirring for 0.5 hour. Filtered to obtain an optical purity of 98.7%e.The D-malate salt of (S)-3-amino-1-butanol.The above-mentioned recrystallized D-malate salt of (S)-3-amino-1-butanol having an optical purity of 98.7% ee was suspended in 150 ml of anhydrous ethanol, and the temperature was raised to reflux. After the system was dissolved, the temperature was slowly lowered. The solids gradually precipitated, dropped to room temperature, incubated for 1 to 1.5 hours while stirring, and continued to cool down to 5 to 10C for half an hour, filtered by suction, and vacuum dried at 50C to a constant weight to give an optical purity of 99.4% ee.(S). D-malate salt of 3-amino-1-butanol.The above-mentioned recrystallized D-malate salt of (S)-3-amino-1-butanol having an optical purity of 99.4%ee was suspended in 120 ml of absolute ethanol, and the temperature was raised to reflux. After the system was dissolved, the temperature was gradually lowered. Solids gradually precipitated, dropped to room temperature, incubated for 1 to 1.5 hours while stirring, and continued to cool to 5 to 10C for half an hour, filtered, and vacuum dried at 50C to constant weight.50.4 g of D-malate salt with an optical purity of 99.9% ee.(S)-3-amino-1-butanol are obtained,Yield 40.3%.

With the rapid development of chemical substances, we look forward to future research findings about 2867-59-6.

Reference:
Patent; Shanghai Disainuo Pharmaceutical Co., Ltd.; Shanghai Disainuo Chemical Pharmaceutical Co., Ltd.; Yancheng Disainuo Pharmaceutical Co., Ltd.; Shanghai Chuangnuo Pharmaceutical Group Co., Ltd.; Li Jinliang; Zhao Nan; Wu Jun; (10 pag.)CN107793320; (2018); A;,
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