HRID2059846

反应详情

EQUATION

反应方程式

HRID 2059846 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Sodium hydride (0.494 g, 12.3 mmol) was added to a stirred solution of 1-tritylpyrimidine-2,4(1H,3H)-dione (1.75 g, 4.9 mmol) in dry THF (75 mL) at RT. After stirring the mixture at RT for 45 min, 2,4,6-triisopropylbenzene-1-sulfonyl chloride (2.99 g, 9.9 mmol) was added and stirring continued at RT for 2 h. The reaction mixture was poured into a stirred mixture of EtOAc and saturated ammonium chloride solution. The organic layer was dried (MgSO4), concentrated and the residue was subjected to flash chromatography (silica gel/hexane-EtOAc 100:0 to 0:100 gradient) to afford 2-oxo-1-trityl-1,2-dihydropyrimidin-4-yl 2,4,6-triisopropylbenzenesulfonate 4A (1.6 g, 52% yield) as a white solid.

WORKUP

后处理

  1. stirringstirring
  2. waitcontinued at RT for 2 h
  3. dry with materialThe organic layer was dried (MgSO4)
  4. concentrationconcentrated