HRID279994

反应详情

EQUATION

反应方程式

HRID 279994 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3.00 g (0.0117 moles) of N-(4-bromophenyl)-3-oxobutyramide and 6 ml concentrated sulfuric acid was stirred and heated to 95°-100° C. (H2O bath) for 11/2 hours. The resulting solution was poured onto an ice/H2O mixture to yield a white crystalline product. The crystals were collected and taken up in 200 ml absolute ethanol. The volume was reduced to 150 ml followed by chilling; crystals were isolated (0.71 g 25.6%), mp 292°-299° C. Anal. Calcd. for C10H8BrNO: C, 50.45; H, 3.39; N, 5.88; Br, 33.56. Found: C, 50.28; H, 3.44; N, 5.83; Br, 33.68. A TLC of the product on silica showed Rf 0.18 with ethyl acetate eluent.

WORKUP

后处理

  1. customto yield a white crystalline product
  2. customThe crystals were collected
  3. temperatureby chilling
  4. customcrystals were isolated (0.71 g 25.6%), mp 292°-299° C