HRID1056516

反应详情

EQUATION

反应方程式

HRID 1056516 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 EtOH (50 mL, 860 mmol) in EtOAc (390 mL), cooled in an ice/water bath, was slowly added acetyl chloride (55 mL, 770 mmol) over 3 minutes. After 5 minutes the cooling bath was removed, and after stirring for 45 min, the solution was added to tert-butyl 2-(6-(2,4-dimethoxyphenyl)-4-oxo-2-thioxo-3,4-dihydropyrimidin-1(2H)-yl)ethylcarbamate (31.7 g, 77.8 mmol). A suspension formed over time, and after stirring for 5 h, the solid was collected by vacuum filtration, rinsing with EtOAc. The solid was pulled dry and dried further under vacuum to afford 26.6 g (99.3%) of the desired product as a colorless solid.

WORKUP

后处理

  1. customover 3 minutes
  2. customAfter 5 minutes the cooling bath was removed
  3. customA suspension formed over time
  4. stirringafter stirring for 5 h
  5. filtrationthe solid was collected by vacuum filtration
  6. washrinsing with EtOAc
  7. customThe solid was pulled dry
  8. customdried further under vacuum