HRID402811

反应详情

EQUATION

反应方程式

HRID 402811 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4,4-Dimethyl-3,4-dihydro-2H-thiochromene-6-carbaldehyde (449 mg, 2.18 mmol, Example 5-28, Step 2) was dissolved in dichloromethane (22.0 mL) and mCPBA (751 mg, 4.35 mmol) was added in one portion. The reaction mixture was stirred at room temperature for 30 minutes. The mixture was then diluted with dichloromethane, washed with saturated aqueous NaHCO3, saturated aqueous NaCl, dried over Na2SO4, filtered and concentrated under vacuum. The crude mixture was purified by silica gel chromatography eluting with 0-5% MeOH/dichloromethane to afford the desired product as a colorless oil.

WORKUP

后处理

  1. washwashed with saturated aqueous NaHCO3, saturated aqueous NaCl
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated under vacuum
  5. customThe crude mixture was purified by silica gel chromatography
  6. washeluting with 0-5% MeOH/dichloromethane