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HRID1396064

反应详情

EQUATION

反应方程式

HRID 1396064 的结构方程式

REACTANTS

反应物

3
结构：O=C(O)c1cccc(S(=O)(=O)Cl)c1
HCID77641

Benzoic acid, 3-(chlorosulfonyl)-

C7H5ClO4S

结构：CCN(C(C)C)C(C)C
HCID81531

Diisopropylethylamine

C8H19N

结构：CCNC(=N)N1CC(CC)C=N1
HCID178464602

未命名化合物

PRODUCTS

生成物

1
结构：CCNC(=NS(=O)(=O)c1cccc(C(=O)O)c1)N1CC(CC)C=N1
HCID178464649

未命名化合物

收率 4%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：ClCCl
溶剂HCID6344

Dichloromethane

CH2Cl2

PROCEDURE

实验过程

Under N2 atmosphere, 1.0 g 4,N-diethyl-4,5-dihydro-pyrazole-1-carboxamidine was dissolved in 15 mL dry DCM, and 1.14 mL DiPEA and 1.31 g of 3-(chlorosulfonyl)benzoic acid were added. The mixture was stirred overnight at room temperature and evaporated to dryness. The residue was purified by flash chromatography (first column with DCM/MeOH/acetic acid 84:15:1; second column with DCM/MeOH/NH4OH 84:15:1) to yield 0.08 g (4%) of an off-white powder.

WORKUP

后处理

  1. customevaporated to dryness
  2. customThe residue was purified by flash chromatography (first column with DCM/MeOH/acetic acid 84:15:1; second column with DCM/MeOH/NH4OH 84:15:1)