Methylhydrazine → HCID 19102736, compound

HRID 1198515Notes

Reaction equation

HRID 1198515 reaction equation
[C:1]([C:4]1[C:5](=[O:21])[N:6]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:7]2[C:12]([C:13]=1O)=[CH:11][CH:10]=[CH:9][N:8]=2)(=O)[CH3:2].[CH3:22][NH:23][NH2:24]>C(O)(=O)C>[CH3:22][N:23]1[C:13]2[C:12]3[CH:11]=[CH:10][CH:9]=[N:8][C:7]=3[N:6]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[C:5](=[O:21])[C:4]=2[C:1]([CH3:2])=[N:24]1

Participants

4

Reactant 2

HCID 6061MethylhydrazineHCID 54715706HCID 54715706, compound

Product 1

HCID 19102736HCID 19102736, compoundYield 60.1%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

Compound 102 obtained in Example 2, 4.0 g (14.3 millimoles), was suspended in 2.5 ml of glacial acetic acid, and 1.8 ml (34.2 millimoles) of methylhydrazine was added to the suspension. The mixture was heated under reflux for 10 hours. The reaction solution was cooled to room temperature, and the precipitate was collected by filtration and recrystallized from DMF-water to give 2.5 g (yield: 60.1%) of Compound 4.

Workup

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 10 hours
  3. filtrationthe precipitate was collected by filtration
  4. customrecrystallized from DMF-water

Sources & evidence

ORD record
ord-690d462821ff4abbaaaad0c94d9f9fbf
Source dataset
uspto-grants-1994_01
Patent number
US05281610

Reaction notes

Loading…