HRID606474

反应详情

EQUATION

反应方程式

HRID 606474 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 1,1-dimethylethyl {[3-({[(6-cyano-4-oxo-3,4-dihydroquinazolin-2-yl)carbonyl]amino}methyl)phenyl]methyl}carbamate obtained in Reference Example 46 (2.14 g, 4.94 mmol) in ethyl acetate (5 mL) was added 4N hydrogen chloride/ethyl acetate (60 mL), and the mixture was stirred at room temperature for 15 hr. The reaction mixture was concentrated under reduced pressure, and the residue was crystallized from toluene. The obtained crude crystals were suspended in ethyl acetate, and the suspension was stirred under heating for 3 hr to give the title compound as a white powder (1.86 g, 99%).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe residue was crystallized from toluene
  3. customThe obtained crude crystals
  4. stirringthe suspension was stirred
  5. temperatureunder heating for 3 hr