Hydrazine hydrate (1:1) → HCID 178491896, compound

HRID 1013835Notes

Reaction equation

HRID 1013835 reaction equation
[Cl:1][C:2]1[CH:25]=[C:24]([O:26][CH3:27])[CH:23]=[C:22]([Cl:28])[C:3]=1[CH2:4][CH:5]1[CH2:9][CH2:8][N:7]([CH:10]2[CH2:15][CH2:14][C:13](=O)[C:12](=[CH:17][N:18](C)C)[CH2:11]2)[C:6]1=[O:21].O.[NH2:30]N>C(O)C>[Cl:28][C:22]1[CH:23]=[C:24]([O:26][CH3:27])[CH:25]=[C:2]([Cl:1])[C:3]=1[CH2:4][CH:5]1[CH2:9][CH2:8][N:7]([CH:10]2[CH2:15][CH2:14][C:13]3[C:12](=[CH:17][NH:18][N:30]=3)[CH2:11]2)[C:6]1=[O:21]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 67317895HCID 67317895, compound

Product 1

HCID 178491896HCID 178491896, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Dissolve 3-(2,6-Dichloro-4-methoxy-benzyl)-1-(3-dimethylaminomethylene-4-oxo-cyclohexyl)-pyrrolidin-2-one in ethanol (Preparation 24) (50 mL), and hydrazine hydrate (2.6 mL, 54 mmol) stir the resulting orange solution for 3 days at room temp. Concentrate the mixture to dryness, dilute with ethanol (15 mL) and ether (20 mL), cooled to 0° C. and filter to give 3.6 g, 68%, as a tan solid. MS (m/z): 394 (M+1).

Workup

  1. concentrationConcentrate the mixture to dryness
  2. additiondilute with ethanol (15 mL) and ether (20 mL)
  3. temperaturecooled to 0° C.
  4. filtrationfilter
  5. customto give 3.6 g, 68%

Sources & evidence

ORD record
ord-e3e1876108bb493f81cd9e4d89ee9a61
Source dataset
uspto-grants-2011_07
Patent number
US07981918B2

Reaction notes

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