Hydrochloric Acid → HCID 86691670, compound

HRID 2408899Notes

Reaction equation

C(O)C.[NH2:4][C:5]1[C:6]2[C:7]3[C:8](=[N:20][N:21]([CH2:23][C:24]4[C:29]([Cl:30])=[C:28]([O:31][CH3:32])[C:27]([CH3:33])=[CH:26][N:25]=4)[N:22]=2)[CH:9]=[C:10]([CH2:15][C:16]([NH:18][CH3:19])=[O:17])[C:11]=3[CH2:12][S:13][N:14]=1.[ClH:34]>O>[ClH:30].[ClH:34].[NH2:4][C:5]1[C:6]2[C:7]3[C:8](=[N:20][N:21]([CH2:23][C:24]4[C:29]([Cl:30])=[C:28]([O:31][CH3:32])[C:27]([CH3:33])=[CH:26][N:25]=4)[N:22]=2)[CH:9]=[C:10]([CH2:15][C:16]([NH:18][CH3:19])=[O:17])[C:11]=3[CH2:12][S:13][N:14]=1

Participants

Conditions

Temperature: 25 °C

Procedure

Ethanol (29.3 ml) and water (0.74 ml) were added to 2-{4-amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide (1.034 g, 2.243 mmol), and the mixture was then stirred at 25° C. Thereafter, 2 M hydrochloric acid in ethanol (6.73 ml, 13.46 mmol) was added to the reaction mixture, and the resulting mixture was then stirred for 3 hours 45 minutes. Thereafter, the precipitated crystal was filtrated, was then washed with ethanol (5 ml), and was then dried under reduced pressure at 40° C. for 1 hour, so as to obtain the above title compound (1.118 g, 2.155 mmol). Yield: 96%.

Workup

stirringthe resulting mixture was then stirred for 3 hours 45 minutes
filtrationThereafter, the precipitated crystal was filtrated
washwas then washed with ethanol (5 ml)
customwas then dried under reduced pressure at 40° C. for 1 hour

Sources & evidence

ORD record: ord-b99ab6992124479cac3b3dab0e16efe6
Source dataset: uspto-grants-2014_08
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08815880B2

Reaction notes

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