Sulfuric acid magnesium salt (1:1) → HCID 178480145, compound

HRID 908028Notes

Reaction equation

[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][CH:3]1[C:7]1[CH:14]=[CH:13][C:10]([CH:11]=O)=[CH:9][CH:8]=1.[NH2:15][C:16]1[CH:24]=[CH:23][CH:22]=[C:21]2[C:17]=1[CH2:18][O:19][C:20]2=[O:25].[O-]S([O-])(=O)=O.[Mg+2]>CC#N>[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][CH:3]1[C:7]1[CH:14]=[CH:13][C:10](/[CH:11]=[N:15]/[C:16]2[CH:24]=[CH:23][CH:22]=[C:21]3[C:17]=2[CH2:18][O:19][C:20]3=[O:25])=[CH:9][CH:8]=1

Participants

Conditions

Temperature: 120 °C

Procedure

A mixture of 4-(1-methylpyrrolidin-2-yl)benzaldehyde (1.89 g, 10 mmol), 4-aminoisobenzofuran-1(3H)-one (1.49 g, 10 mmol) and MgSO4 (12 g, 100 mmol) in CH3CN (60 mL) was refluxed at 120° C. for 4 days. After a hot filtration, CH3CN was partially removed under reduced pressure and a white precipitate was appeared, the title compound was obtained by a direct filtration (1.3 g, yield 41%) as a white solid. LC-MS (ESI) m/z: 440 (M+1)+.

Workup

filtrationAfter a hot filtration, CH3CN
customwas partially removed under reduced pressure

Sources & evidence

ORD record: ord-d17ccce2838842b796b11b97bc122a9a
Source dataset: uspto-grants-2011_09
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08012976B2

Reaction notes

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