Hydrazine hydrate (1:1) → HCID 13078497, compound

HRID 1704608Notes

Reaction equation

HRID 1704608 reaction equation
C([O:3][C:4]([C:6]([C:12]1[S:13][CH:14]=[CH:15][CH:16]=1)=[N:7][N:8]=[C:9](Cl)[CH3:10])=O)C.O.[NH2:18][NH2:19]>C(O)(C)C>[NH2:18][N:19]1[C:4](=[O:3])[C:6]([C:12]2[S:13][CH:14]=[CH:15][CH:16]=2)=[N:7][N:8]=[C:9]1[CH3:10]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 53839116HCID 53839116, compound

Product 1

HCID 13078497HCID 13078497, compound

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent

Procedure

234 g (0.92 mol) of crude 1-ethoxycarbonyl-4-chloro-4-methyl-1-thien-2-yl-2,3-diazabutadiene were dissolved in 600 ml of isopropanol and 125 g (2.5 mol) of hydrazine hydrate were added at 60° C., whilst stirring. Stirring was continued for 8 hours at 60° C. The reaction solution was concentrated to one-third and water was added. The solid which had precipitated was then filtered off, thoroughly rinsed with water and dried. 125g (65.3% of theory) of 4-amino-3-methyl-6-thien-2-yl-1,2,4-triazin-5-one of melting point 210° C. were obtained.

Workup

  1. stirringStirring
  2. concentrationThe reaction solution was concentrated to one-third and water
  3. additionwas added
  4. customThe solid which had precipitated
  5. filtrationwas then filtered off
  6. washthoroughly rinsed with water
  7. customdried

Sources & evidence

ORD record
ord-c3d3ea94b6d74d7bb5a44e60ebce3d67
Source dataset
uspto-grants-1978_11
Patent number
US04127404

Reaction notes

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