Dimethyl-[2-(3-nitro-pyrrol-1-yl)-ethyl]amine → HCID 66914619、化合物

HRID 1189841ノート

反応式

HRID 1189841 の反応式
[CH3:1][N:2]([CH3:13])[CH2:3][CH2:4][N:5]1[CH:9]=[CH:8][C:7]([N+:10]([O-])=O)=[CH:6]1>[Ni].CO.C1COCC1>[CH3:1][N:2]([CH3:13])[CH2:3][CH2:4][N:5]1[CH:9]=[CH:8][C:7]([NH2:10])=[CH:6]1

参加物

4

反応物 1

HCID 66914587Dimethyl-[2-(3-nitro-pyrrol-1-yl)-ethyl]amine

生成物 1

HCID 66914619HCID 66914619、化合物収率 80.9%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

A suspension of dimethyl-[2-(3-nitro-pyrrol-1-yl)-ethyl]-amine (Step 121.2) (650 mg, 3.55 mmol) and Raney Nickel (300 mg) in MeOH/THF (1:1, v/v; 150 mL) was stirred for 7 h at rt, under a hydrogen atmosphere. The mixture was filtered through a pad of celite and the filtrate was concentrated. The residue was purified by silica gel column chromatography (DCM/MeOH/NH3aq, 98:1:1→93:6:1) to afford 440 mg of the title compound as a red oil. Title compound: ESI-MS: 154.1 [M+H]+; TLC: Rf=0.02 (DCM/MeOH, 9:1).

後処理

  1. filtrationThe mixture was filtered through a pad of celite
  2. concentrationthe filtrate was concentrated
  3. customThe residue was purified by silica gel column chromatography (DCM/MeOH/NH3aq, 98:1:1→93:6:1)

出典と根拠

ORDレコード
ord-fc791de47a654c44a8bfc85452b2d2c6
出典データセット
uspto-grants-2014_03
特許番号
US08674099B2

反応ノート

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