HRID1704818

反应详情

EQUATION

反应方程式

HRID 1704818 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of ethyl 6,7-dihydro-4-oxo-4H-pyrimido[2,1-a]isoquinoline-3-carboxylate (1.81 g., 6.7 mmoles), 1.0 N NaOH (25 ml.) and 95% ethanol was refluxed for 20 l minutes. The resulting solution was cooled and acidified with 1.0 HCl (26 ml.) to precipitate the acid, which was crystallized from 2-methoxyethanol to give colorless crystals: 1.02 g. (63% yield), m.p. 215°-217°. An additional recrystallization from 2-methoxyethanol gave material with m.p. 215.5°-217°.

WORKUP

后处理

  1. temperaturewas refluxed for 20 l minutes
  2. temperatureThe resulting solution was cooled
  3. customto precipitate the acid, which
  4. customwas crystallized from 2-methoxyethanol
  5. customto give colorless crystals
  6. customAn additional recrystallization from 2-methoxyethanol
  7. customgave material with m.p. 215.5°-217°