Category: 22972-63-0

Related Products of 22972-63-0, 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. 22972-63-0 name is 2-(3,5-Dimethoxyphenyl)-2-methylpropanenitrile, This 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.

2-(3,5-dimethoxyphenyl)-2-methylpropanenitrile (10 g, 46.9 mmol, Eq: 1.00) was dissolved in MTBE (50 mL). The clear solution was cooled to 10C and 1 M DIBAL-H in heptane (56.3 mL, 56.3 mmol, Eq: 1.2) was added dropwise over 30 min. The reaction mixture was warmed to 20C over 30 min. After 2 h at 20C, the reaction mixture was added to a cold (0C) mixture of heptane (50 mL) and 2 M aqueous HC1 (100 mL). The water phase was separated and extracted with heptane (50 mL). The organic phases were washed twice sequentially with 2 M aqueous HC1 (2×50 mL), then half saturated aqueous NaHCC>3 (50 mL) and half saturated aqueous NaCl (50 mL). The organic phases were combined, dried over Na2S04, filtered and concentrated under reduced pressure to give 10.3 g of the crude title compound as an oil (97a% GC).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-(3,5-Dimethoxyphenyl)-2-methylpropanenitrile, and friends who are interested can also refer to it.

Reference:
Patent; YISSUM RESEARCH DEVELOPMENT COMPANY OF THE HEBREW UNIVERSITY OF JERUSALEM LTD.; ADAM, Jean-Michel; DOTT, Pascal; HOHLER, Marcus; BURGER, Tanja; TAGLIENTE, Orazio; MISCHLER, Ernst; (49 pag.)WO2018/87767; (2018); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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 22972-63-0 as follows. category: nitriles-buliding-blocks

A solution of DIBAL ([1 M] in toluene) (1 60.9 ml_, 160.9 mmol, 2.5 eq) was added dropwise to a stirred solution of 2-(3,5-Dimethoxy-phenyl)-2-methyl-propionitrile (13.2 g, 64.36 mmol, 1 eq) in dry CH2CI2 (320 ml_) under nitrogen at -78 SC. The reaction mixture was stirred at -78 SC for 1 h. An aqueous solution of potassium sodium tartrate (10% solution in water) was added dropwise and the reaction mixture was warmed to room temperature and stirred vigorously overnight. The solid was filtered through celite and rinsed with CH2CI2, the product was extracted with CH2CI2. The combined organic layers were washed with brine and water, dried over anhydrous MgSC , filtered and the solvent was removed under reduced pressure. The product was purified by chromatography on silica gel (heptane/EtOAc, from 100:0 to 80:20). The desired fractions were collected and concentrated to afford the title product as a colorless oil. (1 1 .6 g, 86.5 %). 1 H NMR (300 MHz, CDC ) d 9.46 (s, 1 H), 6.40 (s, 3H), 3.79 (s, 6H), 1 .43 (s, 6H). LC-MS (ESI+): 209.1 (M+H+); R.T. : 1 .388 min. (HPLC Method E).

According to the analysis of related databases, 22972-63-0, the application of this compound in the production field has become more and more popular.

Some common heterocyclic compound, 22972-63-0, name is 2-(3,5-Dimethoxyphenyl)-2-methylpropanenitrile, molecular formula is C12H15NO2, 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. Formula: C12H15NO2

PREPARATION E 2-Methyl-2-(3,5-dihydroxyphenyl)-5-phenylpentane To a solution of the Grignard reagent prepared from 2-phenylbromoethane (5.5 g.), magnesium (0.8 g.) and dry ether (60 ml.) is added a solution of 2-methyl-2-(3,5-dimethoxyphenyl)propionitrile (2.75 g.) in dry ether (20 ml.). The ether is distilled off and replaced by dry benzene (50 ml.) and the mixture refluxed for 48 hours. It is then decomposed by careful treatment with dilute sulfuric acid and heated on a steam bath for 1 hour. The mixture is then extracted with ether, the extract dried (MgSO4) and concentrated to an oil. Distillation of the oil in vacuo affords 2-methyl-2-(3,5-dimethoxyphenyl)-5-phenyl-3-pentanone; b.p. 168 C./0.2 mm. (Yield: 2.32 g., 60%)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 22972-63-0, its application will become more common.

Reference:
Patent; Pfizer Inc.; US4143139; (1979); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts