Tag: M.W=200-300

Reference of 4654-39-1, 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.4654-39-1, name is 2-(4-Bromophenyl)ethanol, molecular formula is C8H9BrO, molecular weight is 201.06, as common compound, the synthetic route is as follows.

1.31.a. 2-[2-(4-bromo-phenyl)-ethoxy]-tetrahydro-pyran 0.025 g of p-toluenesulphonic acid and 2.575 ml (28.22 mmol) of dihydropyran are added successively to a solution of 4.83 g (24.02 mmol) of 2-(4-bromo-phenyl)-ethanol in 12 ml dichloromethane at 0 C. Then the reaction mixture is stirred for three hours at ambient temperature. The reaction mixture is extracted with sodium hydrogen carbonate solution and the organic phase is dried over sodium sulphate. The purification is carried out by column chromatography on Alox (eluant: cyclohexane/ethyl acetate=8:2). Yield: 37 g (32.8% of theory); C13H17BrO2 (M=285.18); calc.: molar peak (M)+: 284/286 fnd.: molar peak (M)+: 284/286.

Statistics shows that 4654-39-1 is playing an increasingly important role. we look forward to future research findings about 2-(4-Bromophenyl)ethanol.

Reference:
Patent; Boehringer Ingelheim International GmbH; US2004/242572; (2004); A1;,
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Synthetic Route of 78573-45-2, 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.78573-45-2, name is 3-(3-(Trifluoromethyl)phenyl)propan-1-ol, molecular formula is C10H11F3O, molecular weight is 204.19, as common compound, the synthetic route is as follows.

10 kg of dichloromethane was added to a 50 L reactor, and 3-(3-trifluoromethylphenyl)propanol (1 kg, 4.90 mol) and triethylamine (0.59 kg, 5.88 mol) were added in sequence with stirring. The jar was rinsed with 3 kg of dichloromethane. Cool down to -5-10 C, Methanesulfonyl chloride (0.62 kg, 5.39 mol) was slowly added dropwise. The temperature of the reaction system was maintained at -5 to 10 C, and the addition was completed at about 50 to 80 minutes. The incubation was continued until the TLC monitoring reaction was complete and the reaction was completed in about 1 h. 10 kg of water was added under stirring, stirring was continued for 20 min, and the layers were allowed to stand. The organic phase was retained, and the aqueous phase was further extracted with 11 kg of dichloromethane. The organic phase was combined and the aqueous phase was discarded. The organic phase was transferred to a 50 L reactor, cooled to 5-10 C, 10 kg of water was added, stirred for 30 min, allowed to stand for stratification, and the aqueous phase was discarded; the organic phase was washed with 10 kg of 10% NaCl solution, allowed to stand for stratification, and the water phase was discarded. go with. The organic phase was dried over 0.50 kg anhydrous magnesium sulfate and stirred for about 1 h. The magnesium sulfate was filtered off, the reaction kettle was rinsed with 2 kg of dichloromethane and the filter cake was washed, and the organic phases were combined. Transfer the organic phase to the concentrator, Concentrated under reduced pressure to give a yellow oily liquid 1.41kg. HPLC purity: 98.58%.

The chemical industry reduces the impact on the environment during synthesis 78573-45-2, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Jiangsu Yong’an Pharmaceutical Co., Ltd.; Luo Huan; Kang Yanlong; Li Qian; Qiu Chunfang; Liu Kelei; Wang Shuaiwei; (8 pag.)CN109096119; (2018); A;,
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Reference of 60666-70-8 , The common heterocyclic compound, 60666-70-8, name is (2-Bromo-5-chlorophenyl)methanol, molecular formula is C7H6BrClO, 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.

General procedure: A DMF solution (8mL) of the o-substituted aryl iodide (0.36mmol), the o-bromobenzyl alcohol (0.36mmol) and norbornene (34mg, 0.36mmol) was added under nitrogen to a Schlenck-type flask, containing Pd(OAc)2 (4mg, 0.018mmol), the phosphine (0.036mmol), when required, and K2CO3 (124mg, 0.90mmol) or CsOPiv (211mg, 0.90). The reaction mixture was stirred at 105°C for 24h. After cooling to room temperature the organic layer was diluted with EtOAc (20mL), washed twice with water (20mL) and dried over Na2SO4. The solvent was removed under reduced pressure and the resulting residue was purified by flash chromatography on silica gel using mixtures of hexane-EtOAc as eluent.

The synthetic route of 60666-70-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Della Ca, Nicola; Fontana, Marco; Xu, Di; Cremaschi, Mirko; Lucentini, Riccardo; Zhou, Zhi-Ming; Catellani, Marta; Motti, Elena; Tetrahedron; vol. 71; 37; (2015); p. 6389 – 6401;,
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Reference of 135241-08-6, 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 135241-08-6 as follows.

the above-mentioned 4-chloro-1-hydroxy-naphthalene carboxylic acid methyl ester 32g of triflic anhydride 68g were dissolved and stirred at room temperature for 6 hours in 400ml of pyridine. 500ml After adding water, using a separatory funnel, and extracted with toluene 500ml. 3333 Further organic layer was washed with pure water three times, the use of dilute aqueous hydrochloric acid The organic layer was washed three times using aqueous sodium bicarbonate The organic layer was washed three times, then the organic layer was washed with pure water three times. The organic layer was collected and dried over anhydrous magnesium sulfate. After filtration over anhydrous magnesium sulfate, and concentrated using a rotary evaporator to obtain a crude product. 4–1-(((20g( 40% ) The crude product with heptane were recrystallized, thereby obtaining the following 4-chloro-1 – (((trifluoromethyl) sulfonyl) hydroxy) naphthalene carboxylate 20g (yield: 40%)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,135241-08-6, its application will become more common.

Reference:
Patent; JNC Co., Ltd.; Kageyama, Akiko; (341 pag.)KR2015/74015; (2015); A;,
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Reference of 5675-51-4, 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. 5675-51-4, name is 1,12-Dodecanediol, molecular formula is C12H26O2, 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.

To a solution of 1,12-dodecanediol (1.00 g, 4.94 mmol) in toluene (20 mL) was added aqueous HBr (48%, 0.67 mL, 5.33 mmol) and the resulting mixture was refluxed until the diol was completely consumed by TLC monitoring (48 h). The mixture was cooled to room temperature and quenched with 1M NaOH. The resulting mixture was extracted with EtOAc. The combined organic layer was washed with H2O and brine, dried over MgSO4, and evaporated. The resulting residue was purified by column chromatography (SiO2, hexane/EtOAc 3:1) to furnish S1 (1.11 g, 85%) as a pale yellow oil

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 5675-51-4, 1,12-Dodecanediol.

Reference:
Article; Takagi, Ryukichi; Igata, Nao; Yamamoto, Kazuhiro; Kojima, Satoshi; Journal of Organometallic Chemistry; vol. 696; 8; (2011); p. 1556 – 1564;,
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Reference of 2425-28-7, 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.2425-28-7, name is 2-Bromo-1-phenylethan-1-ol, molecular formula is C8H9BrO, molecular weight is 201.0605, as common compound, the synthetic route is as follows.

General procedure: A round-bottom flask was charged with alcohol (2 mmol), CuOTf (0.1 mmol, 0.05 equiv) (S)-5-(pyrrolidin-2-yl)-1H-tetrazole (0.1 mmol, 0.05 equiv), TEMPO (0.1 mmol, 0.05 equiv), t-BuOK (2 mmol, 1 equiv) and DMF (5 ml). The reaction mixture was stirred at 25 C open to air until the completion of the reaction, as monitored by TLC. The mixture was then diluted with CH2Cl2 (20 ml), washed with water, dried over Na2SO4, and evaporated under vacuum to give the crude product, which was purified by column chromatography to give the pure product.

The chemical industry reduces the impact on the environment during synthesis 2425-28-7, I believe this compound will play a more active role in future production and life.

Reference:
Article; Liu, Yangyang; Xie, Aming; Li, Junjian; Xu, Xiao; Dong, Wei; Wang, Boliang; Tetrahedron; vol. 70; 52; (2014); p. 9791 – 9796;,
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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. 722-92-9, name is 2-(4-Aminophenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol, molecular formula is C9H7F6NO, 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. Computed Properties of C9H7F6NO

A solution of 2-(4-aminophenyl)- 1,1, 1,3,3, 3-hexafluoropropan-2-ol (0.88 g, 3.4 mmol), 2-acetamido-4-methylthiazole-5-sulfonyl chloride (0.79 g, 3.1 mmol) in acetone (15 mL) and 2,6-lutidine (0.73 mL, 6.2 mmol) was warmed to 60°C for 18 h. The reaction was judged complete by analytical HPLC (starting materials consumed). The solvent was removed in vacuo, and the crude residue was diluted with EtOAc and aq 1M HC1. The layers were separated, and the organic layer was washed with 1M HC1, sat aq NaHC03, brine, dried (MgS04), and concentrated to give a solid.Trituration with warm Et20/hexanes afforded N-(5-(N-(4-(l,l,l,3,3,3-hexafluoro-2- hydroxypropan-2-yl)phenyl)sulfamoyl)-4-methylthiazol-2-yl)acetamide (1.2 g, 86percent yield) as a light tan solid, >95percent pure as judged by analytical HPLC. A small amount of this was further purified by reverse-phase preparative HPLC to >99percent purity to give a colorless solid. 1H NMR (DMSO-J6, 400MHz) delta 12.5 (s, 1H); 10.8 (s, 1H); 8.6 (s, 1H); 7.60 (d, 2H); 7.25 (d, 2H); 2.30 (s, 3H); 2.15 (s, 3H); 13C NMR (DMSO-J6, 100MHz) delta 170.0, 159.6, 153.0, 139.4, 128.4, 126.8, 124.8, 121.9, 121.7, 120.3, 22.8, 16.3; 19F NMR (DMSO-J6, 376MHz) delta -74.1; HRMS (ESI-orbitrap) Calcd for C15Hi4F6N304S2, 478.0330; Found, 478.0319.

With the rapid development of chemical substances, we look forward to future research findings about 722-92-9.

Reference:
Patent; GRIFFIN, Patrick R.; ROUSH, William R.; KUMAR, Naresh; NUHANT, Philippe; BURRIS, Thomas; SOLT, Laura; WO2011/115892; (2011); A1;,
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Synthetic Route of 60666-70-8, 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. 60666-70-8, name is (2-Bromo-5-chlorophenyl)methanol, molecular formula is C7H6BrClO, 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.

Step 1. ((2-Bromo-5-chlorobenzyl)oxy)(tert-butyl)dimethylsilane. Triethylamine (0.30 mL, 2.15 mmol), DMAP (97 mg, 0.79 mmol) and tert-butyldimethylsilyl chloride (TBSCl; 698 mg, 4.63 mmol) were added to a solution of (2-bromo-5-chlorophenyl)methanol (500 mg, 2.26 mmol) in CH2Cl2 (11.3 mL) at room temperature. After stirring overnight, the reaction mixture was partitioned between saturated aqueous sodium bicarbonate (50 mL) and CH2Cl2 (200 mL). The phases were separated and the aqueous phase was extracted with CH2Cl2 (2*100 mL). The combined organic phase was washed with brine, dried (MgSO4), filtered and concentrated in vacuo.

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 60666-70-8, (2-Bromo-5-chlorophenyl)methanol.

Reference:
Patent; Allergan, Inc.; Ngo, Vinh X.; Old, David W.; Burk, Robert M.; (55 pag.)US9540357; (2017); B1;,
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Electric Literature of 19812-64-7, 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. 19812-64-7, name is Tetradecane-1,14-diol. A new synthetic method of this compound is introduced below.

Synthesis Example D-(25) 1,14-Tetradecandiol (1.5 g) was dissolved in 16.5 ml of cyclohexane, and 57% aqueous hydrobromic acid solution (16.5 ml) was added to this solution. The reaction mixture was refluxed for six hours while stirring. After the reaction, the mixture was extracted three times with diethyl ether. The organic layer was neutralized with saturated sodium hydrogen carbonate solution, washed with saline solution, dried over magnesium sulfate, and filtered, and the solvent was distilled off under reduced pressure. Purification of the residue by silica gel flash chromatography (hexane: ethyl acetate = 7:3) gave 14-bromotetradecan-1-ol as white crystals at a 67% yield. Molecular weight: 292.90 (C14H29BrO) TLC: (hexane-ethyl acetate 7-3) Rf value=0.53 1H-NMR: (300MHz, CDCl3) delta: 1.26 (s large, 20H, -(CH2)10-); 1.56 (qt, 2H, J=7.0Hz, -CH2-); 1.85 (qt, 2H, J=7.1Hz, -CH2-); 3.40 (t, 2H, J=6.9Hz, -CH2-Br); 3.64 (t, 2H, J=6.6Hz, -CH2-O-) 13C-NMR: (75MHz, CDCl3)delta: 25.72; 28.17; 28.75; 29.41-32.80; 32.82; 34.05; 63.08

At the same time, in my other blogs, there are other synthetic methods of this type of compound,19812-64-7, Tetradecane-1,14-diol, and friends who are interested can also refer to it.

Reference:
Patent; Meiji Dairies Corporation; EP1854777; (2007); 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 162358-05-6, name is 2-(4-Octylphenyl)ethanol. This compound has unique chemical properties. The synthetic route is as follows. name: 2-(4-Octylphenyl)ethanol

Example 17 Preparation of 4-octylphenethyl methanesulfonate 2-(4-Octylphenyl)ethanol (53 g) and dichloromethane (500 mL) are charged into a 1 liter three-neck round bottom flask equipped with guard tube and addition funnel. Triethylamine (83.5 g) is added, the mixture is stirred for 30 minutes, then it is cooled to 0 C. Methanesulphonyl chloride (35.2 mL) is added drop-wise at 0 C. and the mass is stirred for 3 hours at room temperature. The mass is diluted with water (700 mL) and the organic layer is separated and the aqueous layer is extracted with dichloromethane (2*250 mL). The combined organic layers is washed with saturated sodium bicarbonate (500 mL) and brine solution (500 mL). The organic layer is separated, dried with sodium sulphate, and concentrated under vacuum to obtain the title compound. Yield: 70 g.

With the rapid development of chemical substances, we look forward to future research findings about 162358-05-6.

Reference:
Patent; DR. REDDY’S LABORATORIES LTD.; Katkam, Srinivas; Sagyam, Rajeswar Reddy; Morthala, Raghavendar Rao; Ireni, Babu; Vinigari, Krishna; Ramdoss, Suresh Kumar; Rangineni, Srinivasulu; Tummala, Arjunkumar; Iqbal, Javed; Oruganti, Srinivas; Kandagatla, Bhaskar; US2014/235895; (2014); A1;,
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