Tag: M.W=0-100

Related Products of 2002-24-6, 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. 2002-24-6, name is 2-Aminoethanol hydrochloride. A new synthetic method of this compound is introduced below.

9-(2′-Hydroxyethylamino)-4-methoxy-1-nitroacridine 4-Methoxy-1-nitro-9-phenoxyacridine (0.346 g) is dissolved in phenol (30 g), ethanolamine hydrochloride (0.12 g) is added and the mixture is heated at 80 C. for 1.5 hour. The reaction mixture is cooled to room temperature, diluted with dry ether (20 ml), slowly poured into dry ether (200 ml) and acidified with ethereal solution of hydrogen chloride. The resulting precipitate is filtered off, washed several times with ether and crystallized from absolute ethanol-ether (5:1) to give 9-(2′-hydroxyethylamino)-4-methoxy-1-nitroacridine monohydrochloride as yellow crystals (0.27 g, 77% yield), m.p. 210-212 C. (decomp.) 1H NMR (for a free base) (d6DMSO): delta10.18 (s, 1 H, NH), 7.78 (d, 1 H, J=7.8 Hz, H-8), 7.67 (d, 1 H, J=8.3 Hz, H-5), 7.47 (t, 1 H, J=7.8 Hz, H-6), 7.36 (d, 1 H, J=8.8 Hz), 7.10 (m, 2 H, H-3, H-7), 4.31 (t, 1 H, J=5.4 Hz, OH), 3.70 (t, 2 H, J=6.4 Hz, H-1′), 3.64 (q, 2 H, J=6.3 Hz, H-2′).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2002-24-6, its application will become more common.

Reference:
Patent; Tiwari, Raj; Miller, Daniel G.; Konopa, Jerzy Kazimierz; Wysocka-Skrzela, Barbara; US2002/37831; (2002); 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. 14320-38-8, name is Cyclopent-3-enol, molecular formula is C5H8O, 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. name: Cyclopent-3-enol

To a solution of 3-cyclopentene-1-ol (7.0 g, 83.0 mmol) and Et3N (14.5 g, 143.0 mmol) in CH2Cl2 (200 mL) was added 4-nitrobenzoyl chloride (18.5 g, 100.0 mmol) as solid in several portions over a period of 30 min. The resulting suspension was stirred at room temperature over night. The precipitate was filtered off and the filtrate was washed with water and brine. The organic layer was dried over MgSO4 and concentrated under reduced pressure. The residue was purified by flash chromatography (Biotage SP1; column 40M; TLC method: n-hexane/ethyl acetate 9/1; Rf=0.50), affording the title product (15.6 g, yield 81%): 1H NMR (500 MHz, CDCl3) delta 8.28 (d, J=8.9 Hz, 2H), 8.20 (d, J=8.9 Hz, 2H), 5.81 (m, 2H), 5.69 (m, 1H), 2.95 (m, 2H), 2.61 (m, 2H).

With the rapid development of chemical substances, we look forward to future research findings about 14320-38-8.

Reference:
Patent; ALI, Amjad; Sebhat, Iyassu K.; Franklin, Cristopher L.; Rupprecht, Kathleen M.; Baker, Robert K.; Nargund, Ravi P.; Yan, Lin; Huo, Pei; Shen, Dong-Ming; Almirante, Nicoletta; Biondi, Stefano; Ferrario, Massimiliano; Nicotra, Alessia; US2010/29678; (2010); A1;,
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Synthetic Route of 2854-16-2, 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. 2854-16-2, name is 1-Amino-2-methylpropan-2-ol. A new synthetic method of this compound is introduced below.

To a solution of V-2 (10 mg, 0.020 mmol) in DMF (1 mL) were added l-amino-2- methylpropan-2-ol (9.13 mg, 0.102 mmol), DIEA (0.036 mL, 0.205 mmol) and HATU (14.01 mg, 0.037 mmol) at rt. The reaction was stirred under argon at rt for 1.5 h. Purification by reverse phase chromatography afforded Example V-3 as white solid (9.0 mg, 98percent). LC-MS (ESI) m/z: 446.1 [M+H]+; XH NMR (500MHz, DMSO-d6) 5 9.18 (br. s., 1H), 8.61 (d, J=4.7 Hz, 1H), 8.54 (s, 1H), 8.21 (br. s., 1H), 8.09 (d, J=8.0 Hz, 1H), 7.88 (d, J=5.0 Hz, 1H), 7.83 (s, 1H), 7.75 (d, J=7.4 Hz, 1H), 7.63 (d, J=8.0 Hz, 1H), 7.53 (s, 1H), 7.50 – 7.45 (m, 1H), 7.45 – 7.38 (m, 1H), 5.52 (q, J=6.2 Hz, 1H), 4.62 – 4.47 (m, 3H), 3.25 (d, J=5.8 Hz, 2H), 1.58 (d, J=6.3 Hz, 3H), 1.10 (s, 6H); Analytical HPLC RT E: 0.99 min, F: 1.27 min.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2854-16-2, 1-Amino-2-methylpropan-2-ol, and friends who are interested can also refer to it.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; QUAN, Mimi L.; HU, Zilun; WANG, Cailan; PATIL, Sharanabasappa; WO2015/2915; (2015); A1;,
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Synthetic Route of 109-83-1 , The common heterocyclic compound, 109-83-1, name is 2-(Methylamino)ethanol, molecular formula is C3H9NO, 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.

PREPARATION I; N(2-hydroxyethyl)-4-methoxy-N,2,6-trimethylbenzene-sulphonamide; A solution of 1.76 g (23.4 mM) of 2-(methylamino)ethanol is prepared in 100 ml of DCM and 5.4 g (53 mM) of triethylamine are added. The mixture is cooled to 0 C. and a solution of 5 g (21.3 mM) of 2,6 dimethyl-4-methoxybenzenesulphonyl chloride in 50 ml of DCM is added progressively. The mixture is then agitated for 3 hours at ambient temperature, and then poured over 50 ml of 0.5 N hydrochloric acid. The organic phase is separated and then washed with water, dried over magnesium sulphate and concentrated under reduced pressure. 5.8 g of the compound sought after are thus obtained as a colourless oil (yield=100%). 1H NMR (300 MHz, DMSO) delta: 6.80 (s, 2H); 4.70 (t, 1H); 3.80 (s, 3H); 3.48 (q, 2H); 3.09 (t, 2H); 2.69 (s, 3H); 2.54 (s, 6H).

The synthetic route of 109-83-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Laboratoires Fournier S.A.; US2006/178360; (2006); A1;,
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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.764-48-7, name is Ethylene Glycol Vinyl Ether, molecular formula is C4H8O2, molecular weight is 88.11, as common compound, the synthetic route is as follows.Safety of Ethylene Glycol Vinyl Ether

General procedure: A dry and argon-flushed 10 mL Schlenk tube, equipped with a stirring bar and septum, wascharged with 2-(vinyloxy)ethanol (5, 132 mg, 1.50 mmol, 1.50 equiv) in Et2O (1.5 mL). Then,iPrMgBr (1.55 mmol, 1.55 equiv) was added dropwise at 25 C. After 5 min of stirring,Sc(OTf)3 (49.2 mg, 0.10 mmol, 0.10 equiv) and aldehyde 6 (1.00 mmol, 1.00 equiv) weresuccessively added and the reaction mixture was stirred at 40 C for the given time. After afull conversion was detected by GC-analysis, sat. aq. NH4Cl (15 mL) was added and theaqueous layer was extracted with EtOAc (3 x 15 mL). The combined organic layers weredried over Na2SO4, filtered and solvent was removed under reduced pressure. Purification viacolumn chromatography (SiO2) afforded expected products 4.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,764-48-7, Ethylene Glycol Vinyl Ether, and friends who are interested can also refer to it.

Reference:
Article; Quinio, Pauline; Kohout, Laura; Roman, Daniela Sustac; Gaar, Jakob; Karaghiosoff, Konstantin; Knochel, Paul; Synlett; vol. 27; 11; (2016); p. 1715 – 1719;,
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Application of 16545-68-9 ,Some common heterocyclic compound, 16545-68-9, molecular formula is C3H6O, 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.

Step 1: 1-bromo-5-cyclopropyloxy-2-methyl-4-nitrobenzene 1-bromo-5-fluoro-2-methyl-4-nitrobenzene (70g , 0.3mol), freshly prepared cyclopropanol diethyl ether complex (23g, ?0.4mol) and N, N- dimethylformamide (260mL) were added into a 500mL reaction flask. Sodium tert-butoxide (35g, 0.36mol) was added slowly thereinto at 0Cand the reaction mixture was stirred at 0C for 1.5 hours. After completion of the reaction, the reaction mixture was poured into ice water slowly, and the precipitated solid was filtered to obtain the crude product. The filter cake was then washed with a lot of water and dried through air to obtain the title compound (yellow solid, 78g, 96%), which may be used directly for the subsequent reaction. (MS: [M+1] none)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,16545-68-9, its application will become more common.

Reference:
Patent; Beijing Pearl Biotechnology Limited Liability Company; DONG, Jiaqiang; ZHONG, Boyu; YUAN, Hongbin; SHI, Quan; CHU, Shaosong; ZHANG, Deyi; ZHANG, Ruihao; (219 pag.)EP3150592; (2017); A1;,
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Application of 110-73-6, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 110-73-6 as follows.

[0284] To the solution of compound of Example 1 (120 mg, 0.136 mmol) and catalytic amount of dimethylaminopyridine in CH2Cl2 (2 mL) at 0 C. was added pyridine (0.20 mL, 2.48 mmol) and diphosgen (0.08 mL, 0.66 mmol). The reaction was warmed to room temperature and stirred for 20 h. 2-(Ethylamino)ethanol (0.2 mL, 2.05 mmol) was added to the reaction and the mixture was stirred for another 16 h before being diluted with ethyl acetate (50 mL). The organic solution was washed with sat. aq. NH4Cl (5 mL¡Á2), sat. aq. NaHCO3 (5 mL) and brine, dried over MgSO4, and concentrated. The crude product was purified by chromatography (silica gel, 94:6:0.3 dichloromethane/methanol/conc. NH4OH). The purified product was dissolved in methanol (5 mL) and stirred at room temperature for 72 h. Concentration and purification by chromatography (silica gel, 92:8:0.3 dichloromethane/methanol/conc. NH4OH) yielded 17 mg (13%) of the title compound. MS 954 (M+H)+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,110-73-6, its application will become more common.

Reference:
Patent; Henninger, Todd C.; Macielag, Mark J.; Marinelli, Brett A.; Zhu, Bin; US2004/18994; (2004); A1;,
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Application of 109-83-1, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 109-83-1 as follows.

Synthesis of the Acid Unit AC-07: 2-[2-[[(4-Methoxy-2,3,6-trimethyl-phenyl)sulfonyl]-methyl-amino]-ethoxy]-acetic acid (AC-07) Stage-1: 2-Methylaminoethanol 1 (1 eq. 79.9 mmol) was dissolved in 500 ml of methylene chloride, and triethylamine (1.2 eq., 95.9 mmol) and the sulfonyl chloride 2 (1.2 eq., 95.9 mmol), dissolved in 60 ml of methylene chloride, were then added in succession. The mixture was stirred at room temperature for 4 h (TLC control). H2O (100 ml) and sat. NaHCO3 solution (100 ml) were then added to the reaction mixture. After separation of the phases, the aqueous phase was extracted 3* with methylene chloride (250 ml). The combined organic phases were dried over Na2SO4, filtered and concentrated. The residue was purified by column chromatography (silica, diethyl ether/hexane 8:2?9:1) to obtain the alcohol 3 (66.3 mmol, 83% yield).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,109-83-1, its application will become more common.

Reference:
Patent; Gruenenthal GmbH; US2009/264400; (2009); A1;,
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Synthetic Route of 109-83-1 ,Some common heterocyclic compound, 109-83-1, molecular formula is C3H9NO, 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 1 N-benzyloxycarbonyl-N-methyl-2-aminoethanol 75 g of 2-methylaminoethanol and 101 g of triethyl amine are mixed with 1000 ml of absolute chloroform. 171 g of chloroformic acid benzyl ester are added dropwise to this solution at about 20 C. The mixture is stirred for 1 hour at room temperature, washed with water, diluted hydrochloric acid and again with water and dried over sodium sulphate. After evaporation of the solvent in vacuo 173 g of oil remain. Infrared (film): 1695 cm-1.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 109-83-1, 2-(Methylamino)ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; A. Nattermann & Cie GmbH; US4565659; (1986); A;,
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Synthetic Route of 3279-95-6, 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. 3279-95-6, name is 2-(Aminooxy)ethanol, molecular formula is C2H7NO2, 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.

A solution of 1 -(6-((6-acetyl-1 H-[1 ,2,3]triazolo[4,5-b]pyrazin-1 -yl)methyl)quinolin-3- yl)ethanone (74 mg, 0.213 mmol) and 2-aminooxy-ethanol (35 mg, 0.45 mmol) in 5 mL of methanol and 0.1 mL of acetic acid was stirred at 40 0C overnight. The solvent was removed under reduced pressure and the residue was diluted with DCM and methanol. The precipitate was collected, washed with DCM, dried to afford the title compound (16 mg, 15%) as a white solid. 1H-NMR (400MHz, DMSO-Cf6) delta ppm 9.31 (s, 1 H), 9.23 (d, 1 H), 8.52 (d, 1 H), 8.03 (d, 1 H), 7.98 (s, 1 H), 7.86 (dd, 1 H), 6.22 (s, 2H), 4.76 (d, 2H), 4.31 (t, 2H), 4.22 (t, 2H), 3.72-3.69 (m, 4H), 2.32 (s, 3H), 2.29 (s, 3H). LCMS (method E): [MH]+ = 465, tR = 4.85 min.

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 3279-95-6, 2-(Aminooxy)ethanol.

Reference:
Patent; NOVARTIS AG; DAI, Miao; FU, Xingnian; HE, Feng; JIANG, Lei; LI, Yue; LIANG, Fang; LIU, Lei; MI, Yuan; XU, Yao-chang; XUN, Guoliang; YAN, Xiaoxia; YU, Zhengtian; ZHANG, Ji, Yue; WO2011/20861; (2011); A1;,
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