Hydrochloric Acid → 3-difluoromethyl-4-(4-methylpiperazin-1-ylmethyl)-N-{4-methyl-3-[4-(5-pyrimidinyl)pyrimidin-2-ylamino]phenyl}benzamide hydrochloride

HRID 13781Notes

Reaction equation

[F:1][CH:2]([F:40])[C:3]1[CH:4]=[C:5]([CH:29]=[CH:30][C:31]=1[CH2:32][N:33]1[CH2:38][CH2:37][N:36]([CH3:39])[CH2:35][CH2:34]1)[C:6]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[C:11]([NH:16][C:17]2[N:22]=[C:21]([C:23]3[CH:24]=[N:25][CH:26]=[N:27][CH:28]=3)[CH:20]=[CH:19][N:18]=2)[CH:10]=1)=[O:7].[ClH:41]>C(O)C>[ClH:41].[F:40][CH:2]([F:1])[C:3]1[CH:4]=[C:5]([CH:29]=[CH:30][C:31]=1[CH2:32][N:33]1[CH2:38][CH2:37][N:36]([CH3:39])[CH2:35][CH2:34]1)[C:6]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[C:11]([NH:16][C:17]2[N:22]=[C:21]([C:23]3[CH:28]=[N:27][CH:26]=[N:25][CH:24]=3)[CH:20]=[CH:19][N:18]=2)[CH:10]=1)=[O:7]

Participants

Conditions

Temperature: 70 °C

Procedure

2.66 g of 3-difluoromethyl-4-(4-methylpiperazin-1-ylmethyl)-N-{4-methyl-3-[4-(5-pyrimidinyl)pyrimidin-2-ylamino]phenyl}benzamide (Example 1) was suspended in 26 ml of ethanol and 4.88 ml of 1 N hydrochloric acid was added thereto, and then the mixture was stirred with heating in a hot bath at 70° C. and dissolved. The solvent was distilled off under reduced pressure, and then the crude crystals were washed with ethanol to obtain 2.80 g of the objective compound.

Workup

dissolutiondissolved
distillationThe solvent was distilled off under reduced pressure
washthe crude crystals were washed with ethanol

Sources & evidence

ORD record: ord-f50f57487ad14b86ad99b7996bff5958
Source dataset: uspto-grants-2010_06
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07728131B2

Reaction notes

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