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2-(5-Chloro-7-nitroindolin-1-yl)benzamide → 2-(5-Chloro-7-aminoindolin-1-yl)benzamide

HRID 34338
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인쇄 미리보기

반응식

HRID 34338 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[C:9]([N+:11]([O-])=O)[CH:10]=1)[N:7]([C:14]1[CH:22]=[CH:21][CH:20]=[CH:19][C:15]=1[C:16]([NH2:18])=[O:17])[CH2:6][CH2:5]2>CN(C)C=O.C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[C:9]([NH2:11])[CH:10]=1)[N:7]([C:14]1[CH:22]=[CH:21][CH:20]=[CH:19][C:15]=1[C:16]([NH2:18])=[O:17])[CH2:6][CH2:5]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 138233492-(5-Chloro-7-nitroindolin-1-yl)benzamide

생성물 1

HCID 138232702-(5-Chloro-7-aminoindolin-1-yl)benzamide수율 119.3%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6228Dimethylformamide용매

실험 절차

To the solution of 2-(5-chloro-7-nitroindolin-1-yl)benzamide of Example 1b (10 gm, 26.5 mmoles) in dimethylformamide (DMF) [100 ml] and ethanol (100 ml) was added 1% Pt/carbon (2.0 gm). The mixture was shaken under hydrogen (59 psi) for 41/2 hours. The mixture was then filtered under nitrogen and concentrated to remove solvent at 55° C. and high vacuum to give a solid (9.1 gm). Recrystallization from chloroform twice afforded 2-(5-chloro-7-aminoindolin-1-yl)benzamide, (4.3 gm, 47.3%), m.p. 199°-201° C. dec.

후처리

  1. filtrationThe mixture was then filtered under nitrogen
  2. concentrationconcentrated
  3. customto remove solvent at 55° C.

출처 및 근거

ORD 기록
ord-5f948ac41b9445e7bc809fe917270260
출처 데이터셋
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04761412

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