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HRID1198658

反应详情

EQUATION

反应方程式

HRID 1198658 的结构方程式

REACTANTS

反应物

2
结构：NN.O
HCID24654

Hydrazine hydrate (1:1)

H6N2O

结构：CSC(=S)NCc1ccc(-c2ccccc2C(=O)OC(C)(C)C)cc1
HCID10339332

1,1-Dimethylethyl 4′-[[[(methylthio)thioxomethyl]amino]methyl][1,1′-biphenyl]-2-carboxylate

C20H23NO2S2

PRODUCTS

生成物

1
结构：CC(C)(C)OC(=O)c1ccccc1-c1ccc(CNC(=S)NN)cc1
HCID10338402

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CCO
溶剂HCID702

Ethanol

C2H6O

PROCEDURE

实验过程

A mixture of 1.53 g (4.1 mmole) of methyl N-[[2'-(t-butoxycarbonyl)biphenyl-4-yl]methyl]dithiocarbamate, 796 μl (820 mg, 16.4 mmole) of hydrazine hydrate, and 10 ml of absolute ethanol was stirred at reflux under N2. After 2 hours the resulting solution was cooled and concentrated. The residual oil was chromatographed on a column of silica gel (elution with 99:1 and the 98:2 CH2Cl2) to give (after concentration and vacuum-drying) 1.15 g (79%) of a stiff, white foam, mp>45° C. (gradual); homogeneous by TLC in 19:1 CH2Cl2 -MeOH; mass spectrum (FAB) m/e 358 (M+1)+.

WORKUP

后处理

  1. temperatureat reflux under N2
  2. temperatureAfter 2 hours the resulting solution was cooled
  3. concentrationconcentrated
  4. customThe residual oil was chromatographed on a column of silica gel (
  5. washelution with 99:1
  6. customthe 98:2 CH2Cl2) to give
  7. concentration(after concentration and vacuum-drying) 1.15 g (79%) of a stiff, white foam, mp>45° C. (gradual)