HRID527358

反应详情

EQUATION

反应方程式

HRID 527358 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-(4-(S-methylsulfonimidoyl)benzyl)isoindoline-1,3-dione (preparation 17b, 2.50 g, 7.95 mmol) and triethylamine (2.2 mL, 16 mmol) in dichloromethane (20 mL) is cooled at 0° C. and treated with methanesulfonyl chloride (620 μL, 8.0 mmol). The mixture is stirred at this temperature for 1.5 h and then washed with water. The organic layer is concentrated under reduced pressure, and the residue is suspended in a mixture of methanol and water. The precipitate is filtered, washed with water, and dried. Yield: 273 mg (8% of theory); ESI mass spectrum: [M+H]+=393, r.t. HPLC: 0.44 min (X012_S01).

WORKUP

后处理

  1. washwashed with water
  2. concentrationThe organic layer is concentrated under reduced pressure
  3. additionthe residue is suspended in a mixture of methanol and water
  4. filtrationThe precipitate is filtered
  5. washwashed with water
  6. customdried
  7. custom=393, r.t
  8. custom0.44 min (X012_S01)