Hydrazine hydrate (1:1) → 147508-06-3

HRID 1198513Notes

Reaction equation

HRID 1198513 reaction equation
[C:1]([C:9]1[C:10](=[O:26])[N:11]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:12]2[C:17]([C:18]=1O)=[CH:16][CH:15]=[CH:14][N:13]=2)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[NH2:28][NH2:29]>C(O)(=O)C>[C:2]1([C:1]2[C:9]3[C:10](=[O:26])[N:11]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=4)[C:12]4[N:13]=[CH:14][CH:15]=[CH:16][C:17]=4[C:18]=3[NH:29][N:28]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

4

Procedure

850 mg (2.5 millimoles) of Compound 101 was suspended in 5 ml of glacial acetic acid, and 0.26 ml (5.5 millimoles) of hydrazine monohydrate was added to the suspension. The mixture was heated under reflux for 5 hours and the reaction mixture was cooled to room temperature. The precipitate was collected by filtration, and recrystallized from DMF-water to obtain 440 mg (yield 52.4%) of Compound 1.

Workup

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 5 hours
  3. filtrationThe precipitate was collected by filtration
  4. customrecrystallized from DMF-water

Sources & evidence

ORD record
ord-0a1b44f5768740249712ddde234ff4e6
Source dataset
uspto-grants-1994_01
Patent number
US05281610

Reaction notes

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