HRID236231

反应详情

EQUATION

反应方程式

HRID 236231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7.7 g (0.029 mol) 2-chloro-6-phenylbenzenesulfonamide, 3.6 ml (0.032 mol) n-butylisocyanate and 4.1 g (0.03 mol) potassium carbonate was heated in 80 ml dry acetonitrile for 18 hours at reflux. The solvent was evaporated and the residue treated with 1N HCl and ethyl acetate and the insoluble solids were collected, washed with water and then ether. Additional material was obtained from the organic phase of the filtrate to afford a total of 10 g of the title compound, m.p. 184°-186°. NMR (90 MHz, CDCl3), 0.9 (CH3, t, br), 1.4 (4H, m), 3.05 (q, J=7 Hz, 2H), 5.9 (t, br, NH), 7.2-7.6 (m, 8H) ppm.

WORKUP

后处理

  1. temperatureat reflux
  2. customThe solvent was evaporated
  3. additionthe residue treated with 1N HCl and ethyl acetate
  4. customthe insoluble solids were collected
  5. washwashed with water
  6. customAdditional material was obtained from the organic phase of the filtrate