HRID330536

反应详情

EQUATION

反应方程式

HRID 330536 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3,5-dinitrobenzensulfonyl chloride (4.6 g, 17.3 mmol) in dry tetrahydrofuran (130 mL) was added oer 50 min. to a cooled, stirred solution of N,N-dimethyl ethylenediamine (4.0 mL, 34.6 mmol) in tetrahydrofuran (100 mL). After stirring at room temperature overnight, tetrahydrofuran was removed under reduced pressure and the residue flash chromatographed over silica gel. The sulfonamide (5.1 g) was eluted with 5% methanol- 95% chloroform and purified as the hydrochloride salt, mp 238°-40°.

WORKUP

后处理

  1. customtetrahydrofuran was removed under reduced pressure
  2. customthe residue flash chromatographed over silica gel
  3. washThe sulfonamide (5.1 g) was eluted with 5% methanol- 95% chloroform
  4. custompurified as the hydrochloride salt, mp 238°-40°