反应详情

温度

85 °C

(3-Bromo-4-cyanophenyl)acetic acid (1.0 g, 4.2 mmol) was dissolved in methanol (20 mL), and thionyl chloride (0.5 mL) was added drop wise to the solution. The reaction was heated to 85° C. for 4 h. Then it was cooled to room temperature and evaporated to dryness in vacuo. The residue was partitioned between ethyl acetate and sat. NaHCO3. The organic layer was dried over MgSO4, filtered, and the filtrate was evaporated to dryness under reduced pressure to yield the crude title compound as an off white solid. 1H NMR (500 MHz, CDCl3): δ 7.07 (d, J=7.07 Hz, 1H), 7.00-6.97 (m, 2H), 3.74 (s, 3H), 3.73 (s, 2H). LC-MS (IE, m/z): 195.2 [(M+1)−CO2CH3]+.

1. temperatureThen it was cooled to room temperature
2. customevaporated to dryness in vacuo
3. customThe residue was partitioned between ethyl acetate and sat. NaHCO3
4. dry with materialThe organic layer was dried over MgSO4
5. filtrationfiltered
6. customthe filtrate was evaporated to dryness under reduced pressure