HRID1927553

反应详情

EQUATION

反应方程式

HRID 1927553 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Methyl (2S,4S)-1-BOC-4-[(4,4-dimethylcyclohexyl)amino]pyrrolidine-2-carboxylate (1.01 g, 2.84 mmol) obtained in Step A, was dissolved in pyridine (5 mL), and Ac2O (1.34 mL, 14.20 mmol) was added thereto at room temperature. The reaction solution was heated to 90° C. and was stirred for 2 hours. After the reaction was completed, CuSO4.5H2O aqueous solution was added and the solution was extracted with EtOAc. The extracted organic solution was dried over MgSO4 and concentrated in vacuo. The obtained residue was purified by column chromatography (eluent: EtOAc/Hex=1/1) to give the title compound (0.98 g, 87%).

WORKUP

后处理

  1. customat room temperature
  2. extractionthe solution was extracted with EtOAc
  3. dry with materialThe extracted organic solution was dried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe obtained residue was purified by column chromatography (eluent: EtOAc/Hex=1/1)