Methylhydrazine → HCID 67128179, compound

HRID 241561Notes

Reaction equation

HRID 241561 reaction equation
[CH3:1][NH:2][NH2:3].CN(/[CH:7]=[C:8]1\[C:9](=O)[CH2:10][N:11]([C:13]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:12]\1)C>C(O)C>[CH3:1][N:2]1[C:9]2[CH2:10][N:11]([C:13]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)([C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=3)[C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH2:12][C:8]=2[CH:7]=[N:3]1

Participants

4

Reactant 2

HCID 6061MethylhydrazineHCID 57450660HCID 57450660, compound

Product 1

HCID 67128179HCID 67128179, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A solution of methyl hydrazine (0.11 mL) and (4Z)-4-[(dimethylamino)methylene]-1-tritylpyrrolidin-3-one (678 mg) in ethanol (5 mL) was heated at 84° C. in a sealed tube for 3 h. Solvent was removed under reduced pressure and the residue was purified on a Biotage Horizon® system (silica, 5% methanol/0.5% concentrated ammonium hydroxide/94.5% dichloromethane) to yield 1-methyl-5-trityl-1,4,5,6-tetrahydropyrrolo[3,4-c]pyrazole.

Workup

  1. customSolvent was removed under reduced pressure
  2. customthe residue was purified on a Biotage Horizon® system (silica, 5% methanol/0.5% concentrated ammonium hydroxide/94.5% dichloromethane)

Sources & evidence

ORD record
ord-3207caaf9eef4f4691f116e209d25e3d
Source dataset
uspto-grants-2014_02
Patent number
US08653059B2

Reaction notes

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