HRID1665002

反应详情

EQUATION

反应方程式

HRID 1665002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of 1-(5-bromo-2-thienyl)-methanamine (0.5 g) in dichloromethane (8 mL) were added 2-(trifluoromethyl)-benzenesulfonyl chloride (0.67 g) and N-ethyl-diisopropylamine (0.37 g) at 0° C. After stirring for 10 min, the ice bath was removed and the mixture was stirred for 40 min. The reaction mixture was diluted with dichloromethane and washed with 0.5 M HCl and with water. The organic phase was dried (MgSO4), filtered and concentrated. The residue was suspended in cyclohexane. The solid was collected by filtration and dried to give N-(5-bromo-thiophen-2-ylmethyl)-2-trifluoromethyl-benzenesulfonamide (0.596 g) as a colorless solid. MS: 417.1 ([M+NH4]+)

WORKUP

后处理

  1. customthe ice bath was removed
  2. stirringthe mixture was stirred for 40 min
  3. additionThe reaction mixture was diluted with dichloromethane
  4. washwashed with 0.5 M HCl and with water
  5. dry with materialThe organic phase was dried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. filtrationThe solid was collected by filtration
  9. customdried