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HRID1857826

反应详情

EQUATION

反应方程式

HRID 1857826 的结构方程式

REACTANTS

反应物

3
结构：CCCCN=C=O
HCID8110

Butyl isocyanate

C5H9NO

结构：O=C([O-])[O-].[K+].[K+]
HCID11430

Potassium Carbonate

CK2O3

结构：CC(C)OC(=O)c1ccc(Cl)cc1S(N)(=O)=O
HCID13564712

未命名化合物

PRODUCTS

生成物

1
结构：CCCCNC(=O)NS(=O)(=O)c1cc(Cl)ccc1C(=O)OC(C)C
HCID13564713

未命名化合物

收率 49.5%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CCC(C)=O
溶剂HCID6569

Methyl ethyl ketone

C4H8O

PROCEDURE

实验过程

A mixture of 1063.4 g of isopropyl 2-(aminosulfonyl)-4-chlorobenzoate, 590.4 g of n-butyl isocyanate and 590.4 g of K2CO3 in 10.8 liters of 2-butanone are heated under reflux overnight. After cooling to room temperature, the reaction mixture is in each case poured into 10 liters of ice-water. The aqueous phase is extracted with 9 liters of methylene chloride. The aqueous phase is acidified to pH 1.0 using concentrated HCl, and the resulting precipitate is filtered off. After drying, 714.6 g of isopropyl 2-[N-(N-butylaminocarbonyl)aminosulfonyl]-4-chlorobenzoate (44% of theory) of melting point 129-132° C. are obtained.

WORKUP

后处理

  1. temperatureare heated
  2. temperatureunder reflux overnight
  3. extractionThe aqueous phase is extracted with 9 liters of methylene chloride
  4. filtrationthe resulting precipitate is filtered off
  5. customAfter drying