HCID 67342783, 화합물 → HCID 67343959, 화합물

HRID 1257750노트

반응식

HRID 1257750 반응식
[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][CH2:14][C:13]([NH:18][C:19]2[C:24]([N+:25]([O-])=O)=[CH:23][N:22]=[C:21]3[N:28]([S:31]([C:34]4[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=4)(=[O:33])=[O:32])[CH:29]=[CH:30][C:20]=23)([CH3:17])[CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C(OCC)(=O)C.[Ni]>[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][CH2:14][C:13]([NH:18][C:19]2[C:24]([NH2:25])=[CH:23][N:22]=[C:21]3[N:28]([S:31]([C:34]4[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=4)(=[O:33])=[O:32])[CH:29]=[CH:30][C:20]=23)([CH3:17])[CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 1

HCID 67342783HCID 67342783, 화합물

생성물 1

HCID 67343959HCID 67343959, 화합물수율 100.2%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 3-(1-Benzene sulfonyl-5-nitro-1H-pyrrolo[2,3-b]pyridin-4-ylamino)-3-methyl-piperidine-1-carboxylic acid benzyl ester (400 mg, 0.73 mmol) and Raney Ni (1.0 g) in ethyl acetate (20 mL) was hydrogenated at 25° C. for 1.5 hours. The mixture was filtered through Celite, thoroughly washing the filter cake with methanol. The filtrate and washings were combined and concentrated under vacuum to give about 380 mg (100%) of 3-(5-Amino-1-benzenesulfonyl-1H-pyrrolo[2,3-b]pyridin-4-ylamino)-3-methyl-piperidine-1-carboxyli c acid benzyl ester without further purification. LCMS (Method J, ESI): RT=1.04 min, m+H=519.8.

후처리

  1. filtrationThe mixture was filtered through Celite
  2. washthoroughly washing the filter cake with methanol
  3. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-c2293c3ea7eb46db831007e6516e3cd4
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08461328B2

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