Hydrazine hydrate (1:1) → HCID 21190683, compound

HRID 1068948Notes

Reaction equation

HRID 1068948 reaction equation
[C:1]([NH:8][CH2:9][C:10]1[CH:11]=[C:12]([NH:16][C:17](SC)=[C:18]([C:21]#[N:22])[C:19]#[N:20])[CH:13]=[CH:14][CH:15]=1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].O.[NH2:26][NH2:27]>CO>[NH2:20][C:19]1[NH:27][N:26]=[C:17]([NH:16][C:12]2[CH:13]=[CH:14][CH:15]=[C:10]([CH2:9][NH:8][C:1]([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2])[CH:11]=2)[C:18]=1[C:21]#[N:22]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 21190620HCID 21190620, compound

Product 1

HCID 21190683HCID 21190683, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of 145.4 g (422 mmol) of 3-[3-(N-Boc-aminomethyl)-phenylamino]-2-cyano-3-methylmercapto-acrylonitrile, 21.96 ml (443 mmol) of hydrazine hydrate and 1000 ml of methanol is heated under reflux for 2 hours and then concentrated by evaporation in vacuo, yielding 5-amino-[3(N-Boc-aminomethyl)-phenylamino]4-cyano-pyrazole; TLC-Rf=0.28 (methylene chloride/methanol [9:1]).

Workup

  1. temperatureis heated
  2. temperatureunder reflux for 2 hours
  3. concentrationconcentrated by evaporation in vacuo

Sources & evidence

ORD record
ord-8930110d056e410189ada73072ed8239
Source dataset
uspto-grants-2001_06
Patent number
US06251911B1

Reaction notes

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