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 → 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
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>O>[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]=1Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Procedure
Water (20 mL) was 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 monohydrochloride (which had been obtained by the same operations as those in the method described in the above Reference Example 2) (505 mg, 1.047 mmol), and the resulting mixture was then stirred at room temperature for 3 hours. Thereafter, a precipitate was collected by filtration, and was then air-dried at room temperature for 3 days, so as to obtain the above title compound as crystal P (426 mg, 0.883 mmol). Yield: 84%.
Workup
- customhad been obtained by the same operations as those in the method
- filtrationThereafter, a precipitate was collected by filtration
- customwas then air-dried at room temperature for 3 days
Sources & evidence
- ORD record
- ord-e98c5e7f2c754beebfa8cbf23d4f9be7
- Source dataset
- uspto-grants-2014_09
- Patent number
- US08846703B2
Reaction notes
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