HRID532486

反应详情

EQUATION

反应方程式

HRID 532486 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To 7-bromo-4-chlorothieno[3,2-d]pyrimidine obtained in Step 1-3) of Preparation Example 1, t-butyl 4-hydroxypiperidine-1-carboxylate, K2CO3 and N,N-dimethylformamide were added, and stirred at 100° C. for 12 hours in a hermetically sealed reactor. The reaction mixture was cooled to room temperature, extracted with ethyl acetate and distilled water, and the organic layer thus obtained was washed with water and a saline solution. Subsequently, the washed organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure to obtain the title compound.

WORKUP

后处理

  1. additionwere added
  2. temperatureThe reaction mixture was cooled to room temperature
  3. extractionextracted with ethyl acetate
  4. distillationdistilled water
  5. customthe organic layer thus obtained
  6. washwas washed with water
  7. dry with materialSubsequently, the washed organic layer was dried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure