HRID655249

反应详情

EQUATION

反应方程式

HRID 655249 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of (3-bromo-5,7-difluoro-quinolin-6-yl)-acetic acid methyl ester (10.0 g, 31.6 mmol) in 48 mL of aqueous NaOH (2N) was heated to reflux for 2 hrs then cooled to r.t. The mixture was washed with dichloromethane (50 mL×2) and the aqueous phase acidified with 5N hydrochloric acid to pH 4. The white precipitate was collected via filtration, washed with water and dried. 9.6 g of the title compound was obtained as white powder in 100% yield. 1H NMR (DMSO-d6): δ 12.87 (s, 1H), 9.05 (s, 1H), 8.76 (s, 1H), 7.75˜7.79 (d, 1H), 3.87 (s, 2H).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 2 hrs
  3. washThe mixture was washed with dichloromethane (50 mL×2)
  4. filtrationThe white precipitate was collected via filtration
  5. washwashed with water
  6. customdried