Dichloromethane → HCID 19390523, compound

HRID 617007Notes

Reaction equation

HRID 617007 reaction equation
[CH2:1]([O:3][C:4]([NH:6][NH:7][CH:8]([CH3:10])[CH3:9])=[O:5])[CH3:2].C(=O)(O)[O-].[Na+].C(Cl)Cl.[N:19]#[C:20]Cl>O>[CH2:1]([O:3][C:4]([NH:6][N:7]([CH:8]([CH3:10])[CH3:9])[C:20]#[N:19])=[O:5])[CH3:2]

Participants

6

Reactant 4

HCID 6344DichloromethaneHCID 10477Cyanogen ChlorideHCID 243279ethyl N-(propan-2-ylamino)carbamateHCID 516892Sodium Bicarbonate

Product 1

HCID 19390523HCID 19390523, compoundYield 87.7%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

73.0 g of 2-isopropylhydrazinecarboxylic 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 an hour's stirring, the methylene chloride base is separated, dried over sodium sulphate and the solvent is distilled off in vacuo. There is obtained as residue 75.0 g (87.5% of theory) of 2-isopropyl-2-cyanohydrazinecarboxylic acid ethyl ester as colourless oil.

Workup

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

Sources & evidence

ORD record
ord-9b2990f0431544318ddbd48fceac40cf
Source dataset
uspto-grants-1978_02
Patent number
US04076938

Reaction notes

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