1-Methylpiperazine → HCID 21837641, compound

HRID 1740075Notes

Reaction equation

[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:13](=[O:14])[C:12]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[C:11]([C:20]3[CH:25]=[CH:24][C:23](F)=[CH:22][CH:21]=3)[N:10]2[CH3:27])=[CH:5][CH:4]=1)#[N:2].[CH3:28][N:29]1[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1>C(OCC)(=O)C>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:13](=[O:14])[C:12]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[C:11]([C:20]3[CH:25]=[CH:24][C:23]([N:32]4[CH2:33][CH2:34][N:29]([CH3:28])[CH2:30][CH2:31]4)=[CH:22][CH:21]=3)[N:10]2[CH3:27])=[CH:5][CH:4]=1)#[N:2]

Participants

Conditions

Temperature: 100 °C

Procedure

A liquid mixture of 872 mg of 1-(4-cyanophenyl)-4-ethoxycarbonyl-2-methyl-3-(4-fluorophenyl)-2H-pyrazol-5-one and 2.39 g of N-methylpiperazine was heated at 100° C. for 36 hours with stirring. The reaction solution was cooled to room temperature, and 5 ml of ethyl acetate was added. The precipitated crystals were collected by filtration and dried under reduced pressure to give 519 mg of the title compound as pale yellow crystals.

Workup

temperatureThe reaction solution was cooled to room temperature
filtrationThe precipitated crystals were collected by filtration
customdried under reduced pressure

Sources & evidence

ORD record: ord-3f515851551f4397bb48a83eeed18fbf
Source dataset: uspto-grants-1999_10
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US05968967

Reaction notes

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