HRID1435344

反应详情

EQUATION

反应方程式

HRID 1435344 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of N-methanesulfony-1,2,3,4-tetrahydropyridine (2.18 g, 13.52 mmol, Example 302) in methylene chloride (30 mL) at 0° C., meta-chloroperoxybenzoic acid (3.94 g, 77%, 17.5 mmol, Aldrich) in 20 mL of methylene chloride was added and the mixture was stirred for 30 minutes. An additional 600 mg of meta-chloroperoxybenzoic acid was added and the mixture was stirred for 6 hours. The reaction was quenched with 30% sodium thiosulfate solution and the mixture was extracted with methylene chloride. The extracts were combined, washed with 5% sodium carbonate and dried with MgSO4. The solvent was removed to give the desired product as a white solid. 2.40 g, 100%. The compound was used directly for the next step.

WORKUP

后处理

  1. stirringthe mixture was stirred for 6 hours
  2. customThe reaction was quenched with 30% sodium thiosulfate solution
  3. extractionthe mixture was extracted with methylene chloride
  4. washwashed with 5% sodium carbonate
  5. dry with materialdried with MgSO4
  6. customThe solvent was removed