HRID606433

反应详情

EQUATION

反应方程式

HRID 606433 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5-[({[3′-(aminomethyl)biphenyl-4-yl]methyl}sulfonyl)methyl]-2,4-dihydro-3H-1,2,4-triazol-3-one obtained in Reference Example 111 (0.060 g, 0.167 mmol), ethyl 4-oxo-3,4-dihydro-2-quinazolinecarboxylate obtained according to the methods described in Journal of Organic Chemistry (1978), 43(23), 4485-7 and the like (0.024 g, 0.112 mmol) and triethylamine (0.389 mL, 1.12 mmol) in EtOH (3 mL)-DMA (3 mL) was stirred at 90° C. for 24 hr. The reaction mixture was diluted with ethyl acetate, washed with 0.1N hydrochloric acid and saturated brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was crystallized from EtOH-diethyl ether to give the title compound as a pale-yellow powder (0.032 g, 55%).

WORKUP

后处理

  1. customobtained
  2. washwashed with 0.1N hydrochloric acid and saturated brine
  3. dry with materialdried over sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was crystallized from EtOH-diethyl ether