HRID424400

反应详情

EQUATION

反应方程式

HRID 424400 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

4-(4-Ethoxycarbonyl-4,5-dihydro-thiazol-2-yl)-piperidine-1-carboxylic acid tert-butyl ester (1.0 eq, 8.7 mmol) was solved in 160 ml toluene under inert conditions. To this solution MnO2 (15.0 eq, 130 mmol) was added. The reaction was heated to 70° C. under stirring for 5 h. The mixture was filtered over celite and the filtration agent was washed 3 times with 30 ml toluene and ethylacetate. The combined organic layers were distilled in vacuo. The residue was purified by silica gel chromatography using a DCM/MeOH 95:5 gradient. Yield: 30%

WORKUP

后处理

  1. filtrationThe mixture was filtered over celite
  2. washthe filtration agent was washed 3 times with 30 ml toluene and ethylacetate
  3. distillationThe combined organic layers were distilled in vacuo
  4. customThe residue was purified by silica gel chromatography