Dichloromethane → HCID 53744342, compound

HRID 617009Notes

Reaction equation

HRID 617009 reaction equation
[CH2:1]([O:3][C:4]([NH:6][NH:7][CH2:8][CH3:9])=[O:5])[CH3:2].C(=O)(O)[O-].[Na+].C(Cl)Cl.[N:18]#[C:19]Cl>O>[CH2:1]([O:3][C:4]([NH:6][N:7]([CH2:8][CH3:9])[C:19]#[N:18])=[O:5])[CH3:2]

Participants

6

Reactant 4

HCID 6344DichloromethaneHCID 10477Cyanogen ChlorideHCID 242502ethyl 2-ethylhydrazinecarboxylateHCID 516892Sodium Bicarbonate

Product 1

HCID 53744342HCID 53744342, compoundYield 88%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

66.0 g of 2-ethylhydrazinecarboxylic acid ethyl ester and 42.0 g of sodium bicarbonate are stirred into 200 ml of methylene chloride and 400 ml of water. There is then introduced at room temperature in the course of 20 minutes, with continuous stirring, 30.8 g of gaseous cyanogen chloride. After one hour's subsequent stirring, the methylene chloride phase is separated and dried over sodium sulphate, and the solvent is distilled off in vacuo. There is obtained as residue 69.0 g (88% of theory) of 2-ethyl-2-cyano-hydrazinecarboxylic acid ethyl ester as colourless oil.

Workup

  1. customthe methylene chloride phase is separated
  2. dry with materialdried over sodium sulphate
  3. distillationthe solvent is distilled off in vacuo

Sources & evidence

ORD record
ord-72c14ada106e41b9a68d9b7ad05a44f2
Source dataset
uspto-grants-1978_02
Patent number
US04076938

Reaction notes

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