Hydrazine hydrate (1:1) → HCID 15505466, compound

HRID 1602296Notes

Reaction equation

HRID 1602296 reaction equation
[C:1]([C:3](=[C:6]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][CH2:17][CH3:18])=[CH:12][CH:11]=1)SC)[C:4]#[N:5])#[N:2].O.[NH2:20][NH2:21]>CO>[NH2:2][C:1]1[NH:21][N:20]=[C:6]([NH:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][CH2:17][CH3:18])=[CH:12][CH:11]=2)[C:3]=1[C:4]#[N:5]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 1704466HCID 1704466, compound

Product 1

HCID 15505466HCID 15505466, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of 21.5 g (82.9 mmol) of 2-cyano-3-(4-ethoxy-phenylamino)-3-methylmercapto-acrylonitrile, 4.31 ml (87 mmol) of hydrazine hydrate and 110 ml of methanol is heated under reflux for 7 hours and then concentrated by evaporation in vacuo. Recrystallization of the residue from ethyl acetate/hexane yields the title compound; m.p. 166-167° C.

Workup

  1. temperatureis heated
  2. temperatureunder reflux for 7 hours
  3. concentrationconcentrated by evaporation in vacuo
  4. customRecrystallization of the residue from ethyl acetate/hexane

Sources & evidence

ORD record
ord-823a1c2e79f94489a2738828edcd5b50
Source dataset
uspto-grants-1999_11
Patent number
US05981533

Reaction notes

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