1-Phenylpiperazine → 1,3-DIHYDRO-5-(4-PHENYLPIPERAZIN-1-YLMETHYL)-1-METHYL-2H-PYRROLO[2,3-b]PYRIDIN-2-ONE

HRID 964026ノート

反応式

HRID 964026 の反応式
Br[CH2:2][C:3]1[CH:4]=[C:5]2[CH2:11][C:10](=[O:12])[N:9]([CH3:13])[C:6]2=[N:7][CH:8]=1.[CH:14]1[CH:15]=[CH:16][C:17]([N:20]2[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)=[CH:18][CH:19]=1.C(N(CC)CC)C>O1CCOCC1>[C:17]1([N:20]2[CH2:25][CH2:24][N:23]([CH2:2][C:3]3[CH:4]=[C:5]4[CH2:11][C:10](=[O:12])[N:9]([CH3:13])[C:6]4=[N:7][CH:8]=3)[CH2:22][CH2:21]2)[CH:18]=[CH:19][CH:14]=[CH:15][CH:16]=1

参加物

5

反応物 3

HCID 70961-PhenylpiperazineHCID 8471TriethylamineHCID 190792771,3-dihydro-5-bromomethyl-1-methyl-2H-pyrrolo[2,3-b]pyridin-2-one

生成物 1

HCID 190793161,3-DIHYDRO-5-(4-PHENYLPIPERAZIN-1-YLMETHYL)-1-METHYL-2H-PYRROLO[2,3-b]PYRIDIN-2-ONE収率 65%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

1,3-dihydro-5-bromomethyl-1-methyl-2H-pyrrolo[2,3-b]pyridin-2-one from Preparation 18 (0.14 g, 0.6 mmol) is dissolved in dioxane (20 ml) at room temperature and under argon. Phenylpiperazine (0.1 ml, 0.66 mmol, 1.1 equiv.) and triethylamine (0.1 ml, 0.72 mmol, 1.2 equiv.) are added in succession at the same temperature. After 1 hour 30 minutes' reaction, the reaction mixture is concentrated under reduced pressure and the product is purified on a silica column (dichloromethane/methanol: 97:3). The title compound is obtained in the form of a yellow oil in a yield of 65%. ##STR74##

後処理

  1. customAfter 1 hour 30 minutes' reaction
  2. concentrationthe reaction mixture is concentrated under reduced pressure
  3. customthe product is purified on a silica column (dichloromethane/methanol: 97:3)

出典と根拠

ORDレコード
ord-0ed0090054cd42ada634847724161d45
出典データセット
uspto-grants-1998_06
特許番号
US05767128

反応ノート

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