Methylhydrazine → HCID 21454634, compound

HRID 435904Notes

Reaction equation

HRID 435904 reaction equation
[CH3:1][NH:2][NH2:3].[CH3:4][S:5][C:6]1[S:10][C:9]([N:11]=[C:12]=[O:13])=[N:8][N:7]=1.NN>C(Cl)Cl>[CH3:1][N:2]([C:12]([NH:11][C:9]1[S:10][C:6]([S:5][CH3:4])=[N:7][N:8]=1)=[O:13])[NH2:3]

Participants

5

Reactant 3

HCID 6061MethylhydrazineHCID 9321HydrazineHCID 537505795-Methylthio-1,3,4-thiadiazol-2-yl isocyanate

Product 1

HCID 21454634HCID 21454634, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A solution of methylhydrazine (0.3 mole) in methylene chloride (150 ml) is charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and reflux condenser. 5-Methylthio-1,3,4-thiadiazol-2-yl isocyanate dimer (0.1 mole) is then added, with stirring, at room tempertaure. After the addition is completed the reaction mixture is heated at reflux for a period of about 4 hours. After this time the reaction mixture is stripped of solvent and excess hydrazine to yield the desired product 2-methyl-4-(5-methylthio-1,3,4-thiadiazol-2-yl) semicarbazide as the residue.

Workup

  1. customequipped with a mechanical stirrer
  2. temperaturethermometer and reflux condenser
  3. additionAfter the addition
  4. temperatureis heated
  5. temperatureat reflux for a period of about 4 hours

Sources & evidence

ORD record
ord-7834978c3b0045e4adce5003feba2440
Source dataset
uspto-grants-1977_02
Patent number
US04007031

Reaction notes

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