HRID1871964

反应详情

EQUATION

反应方程式

HRID 1871964 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of the 5-(2,4-bis(1,1-dimethylethoxy)pyrimidin-5-yl)-5H-dibenzo[a,d]cyclohepten-5-ol and triethylsilane (64 ml) in dry dichloromethane (400 ml) at 0° C. was added trifluoroacetic acid (150 ml) dropwise over ten minutes. The cooling bath was removed and the solution was stirred at room temperature overnight. Toluene (300 ml) was added and solution was evaporated under vacuum. The residue was azeotroped with toluene (3 times). The oil was treated with diethyl ether and the precipitated product collected as a white powder (44 g).

WORKUP

后处理

  1. customThe cooling bath was removed
  2. additionToluene (300 ml) was added
  3. customsolution was evaporated under vacuum
  4. customThe residue was azeotroped with toluene (3 times)
  5. additionThe oil was treated with diethyl ether
  6. customthe precipitated product collected as a white powder (44 g)