反应 #46232

反应方程式

4-bromobenzene-1-sulfonyl chloride

sodium bicarbonate

1-methylpiperazine

→

required product

1-(4-Bromophenylsulfonyl)-4-methylpiperazine

溶剂

dichloromethane

dichloromethane

反应条件

后处理

1. 1
   其他The phases were separated
2. 2
   干燥the organic layer was dried over magnesium sulfate
3. 3
   其他Evaporation of the solvent under reduced pressure

实验过程

A solution of 4-bromobenzene-1-sulfonyl chloride (256 mg, 1.00 mmol) in 1 mL of dichloromethane was slowly added to a vial (40 mL) containing 5 mL of a saturated aqueous solution of sodium bicarbonate, dichloromethane (5 mL) and 1-methylpiperazine (100 mg, 1.00 mmol). The reaction was stirred at room temperature overnight. The phases were separated and the organic layer was dried over magnesium sulfate. Evaporation of the solvent under reduced pressure provided the required product, which was used in the next step without further purification. ESI-MS m/z calc. 318.0. found 318.9 (M+1)+. Retention time of 1.30 minutes. 1H NMR (300 MHz, CDCl3) δ 7.65 (d, J=8.7 Hz, 2H), 7.58 (d, J=8.7 Hz, 2H), 3.03 (t, J=4.2 Hz, 4H), 2.48 (t, J=4.2 Hz, 4H), 2.26 (s, 3H).

来源