HRID1979972

反应详情

EQUATION

反应方程式

HRID 1979972 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 50 ml. of dimethylsulfoxide (DMSO) was added 1.01 g. (0.021 m.) of 50% sodium hydride in oil. After the initial gas evolution ceased, 2.53 g. (0.0206 m.) of isopropylsulfonamide [prepared according to Duguet, Rec. Trav. Chim., 25, 215 (1906)] was added. The mixture was stirred under a calcium chloride drying tube for ten minutes after which time 4.90 g. (0.020 m.) of 3-fluoro-4-nitrobenzophenone was added, followed by 20 ml. of DMSO. After stirring for five hours at room temperature, the reaction solution was poured into a mixture of ice and 1N hydrochloric acid which was then extracted several times with ethyl acetate. The extracts were combined, washed with water, and dried over magnesium sulfate. The oil remaining after evaporation was triturated with isopropanol to give 6.65 g. (95% yield) of 3-(isopropylsulfonyl)amino-4-nitrobenzophenone as a yellow powder. Crystallization from isopropanol gave pale yellow needles, m.p. about 115°-116° C.

WORKUP

后处理

  1. stirringAfter stirring for five hours at room temperature
  2. extractionwas then extracted several times with ethyl acetate
  3. washwashed with water
  4. dry with materialdried over magnesium sulfate
  5. customafter evaporation
  6. customwas triturated with isopropanol
  7. customto give 6.65 g