HRID520820

反应详情

EQUATION

反应方程式

HRID 520820 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A suspension of 9-oxo-5,6,7,8,9,10-hexahydro-acridine-3-carboxylic acid (VIa) (10 g, 4.1 mmols) in phosphorous oxychloride (50 mL) was heated to 100° C. for 1 h. Reaction completion was monitored by TLC. After completion, the reaction mixture was cooled to 25° C. and excess phosphorous oxychloride was removed under vacuum. The residue was mixed with ice (50 g) and the pH was adjusted to 4-5 with solid sodium bicarbonate. The solid obtained was filtered, washed with water (250 mL) and dried under vacuum to get 9.6 g (88%) of compound (Vila) as a white solid.

WORKUP

后处理

  1. customReaction completion
  2. temperatureAfter completion, the reaction mixture was cooled to 25° C.
  3. customexcess phosphorous oxychloride was removed under vacuum
  4. additionThe residue was mixed with ice (50 g)
  5. customThe solid obtained
  6. filtrationwas filtered
  7. washwashed with water (250 mL)
  8. customdried under vacuum