HRID260457

反应详情

EQUATION

反应方程式

HRID 260457 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-isopropoxyphenylisocyanate in benzene (25 ml) [prepared from 3-isopropoxybenzoic acid (405 mg) in substantially the same manner as described in Method A of Example 1] was added 6-chloro-1,2-dihydro-3-hydroxymethyl-2-methyl-1-oxo-4-phenylisoquinoline (Reference Example 3) (300 mg), and the mixture was heated for 1.5 hours under reflux. The solvent was distilled off. To the residue was added ethyl acetate. This mixture was washed with water, dilute hydrochloric acid, water, an aqueous solution of sodium carbonate and water, successively, followed by drying (Na2SO4). The solvent was distilled off to leave the title compound as colorless crystals (435 mg).

WORKUP

后处理

  1. temperaturethe mixture was heated for 1.5 hours
  2. temperatureunder reflux
  3. distillationThe solvent was distilled off
  4. additionTo the residue was added ethyl acetate
  5. washThis mixture was washed with water, dilute hydrochloric acid, water
  6. dry with materialby drying (Na2SO4)
  7. distillationThe solvent was distilled off