HCID 67342783、化合物 → HCID 67343959、化合物

HRID 1257750ノート

反応式

HRID 1257750 の反応式
[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

参加物

4

反応物 1

HCID 67342783HCID 67342783、化合物

生成物 1

HCID 67343959HCID 67343959、化合物収率 100.2%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-c2293c3ea7eb46db831007e6516e3cd4
出典データセット
uspto-grants-2013_06
特許番号
US08461328B2

反応ノート

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