Hydrazine hydrate (1:1) → HCID 18985860, compound

HRID 2396680Notes

Reaction equation

HRID 2396680 reaction equation
O.[NH2:2][NH2:3].Cl[C:5]1[C:6]2[N:16]=[CH:15][CH:14]=[CH:13][C:7]=2[N:8]=[C:9]([S:11][CH3:12])[N:10]=1>C(O)C>[NH:2]([C:5]1[C:6]2[N:16]=[CH:15][CH:14]=[CH:13][C:7]=2[N:8]=[C:9]([S:11][CH3:12])[N:10]=1)[NH2:3]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 18985854HCID 18985854, compound

Product 1

HCID 18985860HCID 18985860, compoundYield 95.9%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Hydrazine hydrate (13.0 mL (13.3 g, 237 mmol)) was added at ambient temperature with stirring to a mixture of 16.7 g (79 mmol) of 4-chloro-2-methylthiopyrido[3,2-d]pyrimidine in 200 mL of ethanol. There was a slight exotherm and the mixture thickened and then became more mobile again. After 30 min, the volatile components were removed by evaporation under reduced pressure. The residue was diluted with water and the solids were recovered by filtration, washed with ether, and dried to obtain 15.7 g of the title compound as a brown powder melting above 300° C.

Workup

  1. customthe volatile components were removed by evaporation under reduced pressure
  2. additionThe residue was diluted with water
  3. filtrationthe solids were recovered by filtration
  4. washwashed with ether
  5. customdried

Sources & evidence

ORD record
ord-7caae692bb55404a8692bd31f01bf9e2
Source dataset
uspto-grants-1996_02
Patent number
US05494887

Reaction notes

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