Hydrazine hydrate (1:1) → HCID 21190627, compound

HRID 1068958Notes

Reaction equation

HRID 1068958 reaction equation
[C:1]([NH:8][CH2:9][CH2:10][NH:11][C:12](SC)=[C:13]([C:16]#[N:17])[C:14]#[N:15])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].O.[NH2:21][NH2:22]>CO>[NH2:15][C:14]1[NH:22][N:21]=[C:12]([NH:11][CH2:10][CH2:9][NH:8][C:1]([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2])[C:13]=1[C:16]#[N:17]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 21190662HCID 21190662, compound

Product 1

HCID 21190627HCID 21190627, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of 80.81 g (286.4 mol) of 3-[2-(Boc-amino)-ethylamino]-2-cyano-3-methylmercapto-acrylonitrile, 14.9 ml (300.7 mmol) of hydrazine hydrate and 500 ml of methanol is heated under reflux for 4 hours and then concentrated by evaporation in vacuo at about 50° C., yielding 5-amino-3-[2-(Boc-amino)-ethylamino]-4-cyano-pyrazole; TLC-Rf=0.27 (methylene chloride/methanol [9:1]).

Workup

  1. temperatureis heated
  2. temperatureunder reflux for 4 hours
  3. concentrationconcentrated by evaporation in vacuo at about 50° C.

Sources & evidence

ORD record
ord-c14a8d6d4a33454f9362277a345d35bf
Source dataset
uspto-grants-2001_06
Patent number
US06251911B1

Reaction notes

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