HCID 3647008, compound → HCID 86652178, compound

HRID 882993Notes

Reaction equation

[CH2:1]([S:7]([O-:10])(=[O:9])=[O:8])[CH2:2][S:3]([O-:6])(=[O:5])=[O:4].[NH2:11][C:12]1[C:13]2[C:14]3[C:15](=[N:27][N:28]([CH2:30][C:31]4[C:36]([Cl:37])=[C:35]([O:38][CH3:39])[C:34]([CH3:40])=[CH:33][N:32]=4)[N:29]=2)[CH:16]=[C:17]([CH2:22][C:23]([NH:25][CH3:26])=[O:24])[C:18]=3[CH2:19][S:20][N:21]=1>CC(C)=O>[CH2:1]([S:7]([OH:10])(=[O:9])=[O:8])[CH2:2][S:3]([OH:6])(=[O:5])=[O:4].[NH2:11][C:12]1[C:13]2[C:14]3[C:15](=[N:27][N:28]([CH2:30][C:31]4[C:36]([Cl:37])=[C:35]([O:38][CH3:39])[C:34]([CH3:40])=[CH:33][N:32]=4)[N:29]=2)[CH:16]=[C:17]([CH2:22][C:23]([NH:25][CH3:26])=[O:24])[C:18]=3[CH2:19][S:20][N:21]=1

Participants

Conditions

Temperature: 5 °C

Procedure

An acetone solution (50 ml) of ethane-1,2-disulfonate (70 mg, 0.368 mmol) was added at 5° C. to an acetone solution (50 ml) 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 (164 mg, 0.368 mmol). The resulting mixture was stirred at 5° C. for 20 minutes. Thereafter, the reaction solution was left at rest at 5° C. for 18 hours, and it was then stirred at room temperature for 7 hours. Thereafter, the precipitated solid was collected by filtration, and it was then dried under reduced pressure at room temperature for approximately 1 day, so as to obtain the title compound (119 mg, 0.187 mmol).

Workup

waitThereafter, the reaction solution was left at rest at 5° C. for 18 hours
stirringit was then stirred at room temperature for 7 hours
filtrationThereafter, the precipitated solid was collected by filtration, and it
customwas then dried under reduced pressure at room temperature for approximately 1 day

Sources & evidence

ORD record: ord-bdf3e79d283245c3a9bc40c7f5fe1a24
Source dataset: uspto-grants-2012_08
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08236813B2

Reaction notes

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