HRID1374779

反应详情

EQUATION

反应方程式

HRID 1374779 的结构方程式

PROCEDURE

实验过程

7-Benzyloxy-6-bromo-2-methyl-quinolin-4-ol (25.0 g, 72.6 mmol) and phosphorous oxychloride (70 mL, 0.764 mol) were heated 40 min at 130° C. and then cooled down to room temperature. Phosphorous oxychloride was evaporated under high vacuum. Ice water was added and the pH of this solution was adjusted to 9 with ammonium hydroxide. The suspension was extracted with dichloromethane. The combined organic layers were dried under vacuum. 22.8 g of the title compound were obtained. Brown solid, ISP-MS: m/e=364.0 ([M+H]+).

WORKUP

后处理

  1. customPhosphorous oxychloride was evaporated under high vacuum
  2. additionIce water was added
  3. extractionThe suspension was extracted with dichloromethane
  4. customThe combined organic layers were dried under vacuum