HRID1942465

反应详情

EQUATION

反应方程式

HRID 1942465 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To tert-butyl (3R)-3-[{[4-(2-aminoethyl)-2,2-dimethyl-3-oxo-7-(trifluoromethyl)-3,4-dihydro-2H-1,4-benzoxazin-6-yl]carbonyl}(isopropyl)amino]piperidine-1-carboxylate (100 mg) were added methylpropane dithionate (23 mg), triethylamine (0.050 ml) and MeOH (3 ml), and the mixture was stirred at room temperature for 3 hours. After the reaction was complete, water was added to the reaction solution, and the mixture was extracted with ethyl acetate solution. The obtained ethyl acetate solution was washed with water and an aqueous sodium chloride solution, dried over magnesium sulfate, filtered and concentrated. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/2) to give the title compound (90 mg) as a colorless liquid.

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate solution
  2. washThe obtained ethyl acetate solution was washed with water
  3. dry with materialan aqueous sodium chloride solution, dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/2)