Adding a certain compound to certain chemical reactions, such as: 21524-39-0, name is 2,3-Difluorobenzonitrile, belongs to nitriles-buliding-blocks compound, 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 21524-39-0, 21524-39-0
Example 11; Step llA : Compound 11b; To a flame-dried flask, 2,3-difluorobenzonitirle (10 g, 72 mmol) was added along with dry ether (18 mL) and the mixture was allowed to stir at room temperature under nitrogen atmosphere. To the reaction flask, isopropyl Grignard reagent (72 mL, 2M in ether) was added slowly. The reaction mixture was then allowed to reflux (-40 C) for 2 hours. The reaction was then cooled to 0 C and was quenched with a mixture of water (30 mL) and 2N HC1 (60 mL). The biphasic reaction mixture stirred at 50 C for 3 hours then cooled to room temperature. The organic layer was separated and the aqueous phase was extracted with ether (2 x 75 mL). The organic phases were combined and were washed with saturated NaHC03 solution (2 x 100 mL) followed by washing with saturated NaCl solution (100 mL). The organic layer was isolated, dried over anhydrous MgS04, filtered, and evaporated to dryness in vacuo. Difluorophenyl ketone Ila, was recovered in 86% yield (11.6 g, 63 mmol) after purification by column chromatography on silica using 30% hexanes/dichloromethane as the eluent (Rf= 0. 8). Compound lla (11. 6 g, 63 mmol) was dissolved in 1,4-dioxane (63 mL) along with potassium carbonate (17. 5g, 127 mmol) and 1-boc-piperazine (11. 8 g, 63 mmol). The reaction mixture was allowed to reflux for 2 days then cooled to room temperature and filtered to remove potassium carbonate. Solvent from the mother liquor was removed under vacuum and the residue was purified by column chromatography on silica using 10% ethyl acetate/hexanes as the eluent (Rf= 0.3) to give 11b (15.8, 45 mmol, 71% yield). MS: calc. for Cl9H27FN203 : 350.2 ; Found: 351.0 (M+H); retention time: 2.24 minutes; Method info: APCI positive ion scan 100-1000 Frag V = 80; 95% 0.05% TFA/H20 to 95% ACN/0.05% TFA over 2 min, 3.4 min run, ODS-AQ column.
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, 2,3-Difluorobenzonitrile, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; NEUROCRINE BIOSCIENCES, INC.; WO2005/42516; (2005); A2;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts