1-Piperazinecarboxaldehyde → 3-[3-(4-formyl-1-piperazinyl)-1-oxopropyl]-7,11b,12,13-tetrahydro-5H-isoindolo[2,1-b][2]benzazepin-7-one

HRID 53507

반응식

HRID 53507 반응식
Cl[CH2:2][CH2:3][C:4]([C:6]1[CH:24]=[CH:23][C:9]2[CH2:10][CH2:11][CH:12]3[C:21]4[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=4)[C:15](=[O:22])[N:13]3[CH2:14][C:8]=2[CH:7]=1)=[O:5].[CH:25]([N:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1)=[O:26]>>[CH:25]([N:27]1[CH2:32][CH2:31][N:30]([CH2:2][CH2:3][C:4]([C:6]2[CH:24]=[CH:23][C:9]3[CH2:10][CH2:11][CH:12]4[C:21]5[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=5)[C:15](=[O:22])[N:13]4[CH2:14][C:8]=3[CH:7]=2)=[O:5])[CH2:29][CH2:28]1)=[O:26]

참가 물질

3

실험 절차

Using 3.45 g of 3-(3-chloro-1-oxopropyl)-7,11b,12,13-tetrahydro-5H-isoindolo[2,1-b][2]benzazepin-7-one, corresponding to Reference Example 5 Compound No. 1, and 1.4 g of 1-formylpiperazine, the procedure of Example 1 was otherwise repeated to provide about 3.6 g of 3-[3-(4-formyl-1-piperazinyl)-1-oxopropyl]-7,11b,12,13-tetrahydro-5H-isoindolo[2,1-b][2]benzazepin-7-one as a crude oil. This oil was not further purified but directly dissolved in 50 ml of methanol and the solution was refluxed with 50 ml of concentrated hydrochloric acid for 4 hours. After the methanol was distilled off, the residual aqueous solution was adjusted to pH about 10 with 10% aqueous sodium hydroxide solution and the product was extracted into dichloromethane. The extract was washed with water and the solvent was distilled off under reduced pressure to provide 3.1 g of the title compound as a powder melting at 207°-210° C. Elemental analysis for C24H27N3O2

출처 및 근거

ORD 기록
ord-0104847d8211441488c0b6d8376a1a73
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05620973

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