Hydrazine hydrate (1:1) → HCID 178432964, compound

HRID 2200322Notes

Reaction equation

HRID 2200322 reaction equation
O.[NH2:2][NH2:3].[Br:4][C:5]1[CH:6]=[CH:7][C:8]([C:12]#[N:13])=[N:9][C:10]=1[CH3:11]>C(O)C>[Br:4][C:5]1[CH:6]=[CH:7][C:8]([C:12](=[NH:13])[NH:2][NH2:3])=[N:9][C:10]=1[CH3:11]

Participants

4

Conditions

Temperature
50 °C

Procedure

Hydrazine monohydrate (2 equiv) was added to a stirring 1.2 M suspension of 5-bromo-6-methylpicolinonitrile (1 equiv) in ethanol. The reaction mixture was heated to 50° C. for 24 h. The reaction was cooled to room temperature and filtered. The collected solid was washed with ethanol and t-butyl methyl ether. The solid was dried under vacuum to provide the title compound, as a solid. MS (ESI) m/z 228.9 [M]+, 230.9 [M+2]+.

Workup

  1. temperatureThe reaction was cooled to room temperature
  2. filtrationfiltered
  3. washThe collected solid was washed with ethanol and t-butyl methyl ether
  4. customThe solid was dried under vacuum

Sources & evidence

ORD record
ord-c78521767bdc4d6e883e98d42b8f7398
Source dataset
uspto-grants-2016_06
Patent number
US09359364B2

Reaction notes

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