Stannous chloride dihydrate → HCID 117699228, compound

HRID 1049825Notes

Reaction equation

[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1([CH2:16][S:17]([N:20]([C:22]2[CH:27]=[CH:26][C:25]([N:28]3[C:34](=[O:35])[CH2:33][C:32](=[O:36])[NH:31][C:30]4[C:37]5[C:42]([CH:43]=[CH:44][C:29]3=4)=[CH:41][CH:40]=[CH:39][CH:38]=5)=[CH:24][CH:23]=2)[CH3:21])(=[O:19])=[O:18])[CH:15]=[CH:14][CH:13]=[CH:12][CH2:11]1)([O-])=O.O.O.[Sn](Cl)Cl>ClCCl.C(OCC)(=O)C>[NH2:1][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1([CH2:16][S:17]([N:20]([C:22]2[CH:27]=[CH:26][C:25]([N:28]3[C:34](=[O:35])[CH2:33][C:32](=[O:36])[NH:31][C:30]4[C:37]5[C:42]([CH:43]=[CH:44][C:29]3=4)=[CH:41][CH:40]=[CH:39][CH:38]=5)=[CH:24][CH:23]=2)[CH3:21])(=[O:19])=[O:18])[CH:11]=[CH:12][CH:13]=[CH:14][CH2:15]1

Participants

Conditions

Temperature: 30 °C

Procedure

1-(2-Nitrophenyl)-N-[4-(2,4-dioxo-1,2,3,4-tetrahydronaphtho[1,2-b][1,4]diazepin-5-yl)phenyl]phenyl-N-methylmethanesulfonamide (33 mg, 0.062 mmol) mentioned above was dissolved in a mixed solvent of dichloromethane (0.5 mL) and ethyl acetate (1.5 mL), then the solution was added with tin(II) chloride dihydrate (70 mg, 0.310 mmol), and the mixture was stirred at 30° C. for 16 hours. After the disappearance of the starting materials was confirmed, the reaction mixture was treated in a conventional manner to give the title compound (26 mg, yield 31%) as white crystals.

Workup

additionthe reaction mixture was treated in a conventional manner

Sources & evidence

ORD record: ord-d3ba835a57724333bd7f5767e384f1e3
Source dataset: uspto-grants-2016_07
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US09382236B2

Reaction notes

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