Methanesulfonic Acid → N-piperidino-5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-pyrazole-3-carboxamide methanesulfonate

HRID 55361Notes

Reaction equation

[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[N:6]1([NH:12][C:13]([C:15]2[C:19]([CH3:20])=[C:18]([C:21]3[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=3)[N:17]([C:28]3[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][C:29]=3[Cl:35])[N:16]=2)=[O:14])[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1>CC(C)=O>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[N:6]1([NH:12][C:13]([C:15]2[C:19]([CH3:20])=[C:18]([C:21]3[CH:22]=[CH:23][C:24]([Cl:27])=[CH:25][CH:26]=3)[N:17]([C:28]3[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][C:29]=3[Cl:35])[N:16]=2)=[O:14])[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1

Participants

Conditions

Temperature: 0 °C

Procedure

A solution of 0..062 g of methanesulfonic acid in 2 ml of acetone is added dropwise to a solution of 0.30 g of the compound obtained in example 195 in 3 ml of acetone. The white crystals formed upon cooling to 0° C. are filtered off, washed with acetone and dried under vacuum to give 0.30 g of the expected salt. m.p.=218° C.

Workup

customThe white crystals formed
filtrationare filtered off
washwashed with acetone
customdried under vacuum

Sources & evidence

ORD record: ord-7ac373ea448146cb93e358a89d6582a7
Source dataset: uspto-grants-1997_04
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US05624941

Reaction notes

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