Hydrochloric Acid → 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 hydrochloride

HRID 81698Notes

Reaction equation

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

Participants

Conditions

Temperature: 25 °C

Procedure

3 M Hydrochloric acid (0.786 ml, 2.358 mmol) was added to an ethanol (30 ml) suspension of 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 (527.52 mg, 1.183 mmol) while stirring at 25° C., and the mixture was then stirred for 1 hour. Thereafter, the precipitated solid was filtered, was then washed with ethanol (6 ml), and was then dried under reduced pressure at 40° C. for 30 minutes, so as to obtain the above title compound (531.09 g, 1.101 mmol).

Workup

stirringthe mixture was then stirred for 1 hour
filtrationThereafter, the precipitated solid was filtered
washwas then washed with ethanol (6 ml)
customwas then dried under reduced pressure at 40° C. for 30 minutes

Sources & evidence

ORD record: ord-2717f59a547145aabfe0daf6b0cdc8db
Source dataset: uspto-grants-2014_09
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08846703B2

Reaction notes

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