Hydrazine hydrate (1:1) → 1154030-52-0

HRID 1913189Notes

Reaction equation

HRID 1913189 reaction equation
Br[C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([CH3:9])=[CH:4][N:3]=1.O.[NH2:11][NH2:12]>C(O)C>[NH:11]([C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([CH3:9])=[CH:4][N:3]=1)[NH2:12]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 110414352-BROMO-4,5-DIMETHYLPYRIDINE

Product 1

HCID 552791581154030-52-0

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

3.8 g (18.4 mmol, purity 90%) of the compound from Example 20A are initially charged in 12.5 ml of ethanol. 8.9 ml (9.2 g, 183.8 mmol) of hydrazine hydrate are added, and the mixture is reacted in a single-mode microwave oven (CEM Explorer) at 170° C. (100 Watt) for 2 h. The reaction solution is then concentrated, and the residue is taken up in ethyl acetate and washed in each case once with saturated sodium bicarbonate solution and saturated sodium chloride solution. The organic phase is dried over sodium sulfate, filtered and concentrated under reduced pressure.

Workup

  1. customthe mixture is reacted in a single-mode microwave oven (CEM Explorer) at 170° C. (100 Watt) for 2 h
  2. concentrationThe reaction solution is then concentrated
  3. washwashed in each case once with saturated sodium bicarbonate solution and saturated sodium chloride solution
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-7535d233287e4b47817e13f3bf7c4463
Source dataset
uspto-grants-2013_12
Patent number
US08609698B2

Reaction notes

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