Hydrochloride methanol → HCID 68459962, compound

HRID 502906Notes

Reaction equation

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

Participants

Reactant 2

HCID 21893726Hydrochloride methanol

HCID 59428177HCID 59428177, compound

Product 1

HCID 68459962HCID 68459962, compoundYield 72%

Procedure

A mixture of 5,6-difluoro-N-({1-[(4-hydroxytetrahydro-2H-pyran-4-yl)methyl]piperidin-4-yl}methyl)-3-isopropyl-2-oxo-2,3-dihydro-1H-benzimidazole-1-carboxamide (Step 3 of Example 10, 113 mg, 0.242 mmol) and 10% HCl-methanol (5 mL) was stirred for 1 h. Then, the volatile components were removed under reduced pressure and the residue was recrystallized from ethanol-diethyl ether to give 88 mg (72%) of the title compound as a colorless powder.

Workup

customThen, the volatile components were removed under reduced pressure
customthe residue was recrystallized from ethanol-diethyl ether

Sources & evidence

ORD record: ord-2d2f1c0e4a5240e09af144a8b19b0d26
Source dataset: uspto-grants-2010_08
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07776885B2

Reaction notes

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