HRID1702527

反应详情

EQUATION

反应方程式

HRID 1702527 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 22.9 g methyl o-aminosulfonylbenzeneacetate, 13.5 g n-butyl isocyanate, 15.2 g potassium carbonate and 250 ml methyl ethyl ketone was stirred and refluxed for three hours. The reaction mixture was cooled, poured into 1250 g of ice-water, and acidified to pH 1.5 with concentrated HCl. The product was filtered, washed and dried. The crude product was recrystallized from 1-chlorobutane to yield 24.3 g of purified N-(n-butyl)sulfonylurea derivative of methyl o-isocyanatosulfonylbenzeneacetate, m.p. 164°-166° (dec.).

WORKUP

后处理

  1. temperaturerefluxed for three hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationThe product was filtered
  4. washwashed
  5. customdried
  6. customThe crude product was recrystallized from 1-chlorobutane