HRID1437220

反应详情

EQUATION

反应方程式

HRID 1437220 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(2-Hydroxyethyl)piperidine-1-carboxylic acid tert-butyl ester (229 mg) obtained from Referential Example 77 and triethylamine (209 μL) were dissolved in methylene chloride (5 mL) To the resultant solution, methanesulfonyl chloride (116 μL) was added at room temperature, followed by stirring for 30 minutes. The residue obtained by removal through evaporation of the reaction solvent under reduced pressure was partitioned between water and methylene chloride. The organic layer was sequentially washed with water and saturated brine, and then dried over sodium sulfate anhydrate, followed by filtration. The solvent was evaporated under reduced pressure, to thereby give the title compound in the form of crystals (288 mg, 93%).

WORKUP

后处理

  1. additionwas added at room temperature
  2. customThe residue obtained by removal through evaporation of the reaction solvent under reduced pressure
  3. customwas partitioned between water and methylene chloride
  4. washThe organic layer was sequentially washed with water and saturated brine
  5. dry with materialdried over sodium sulfate anhydrate
  6. filtrationfollowed by filtration
  7. customThe solvent was evaporated under reduced pressure