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1-(1-Methyl-4-piperidinyl)piperazine → 4-(1-Methyl-piperidin-4-yl)-piperazine-1-carboxylic acid [3-(2-ethoxy-phenyl)-5-methoxy-2-oxo-2,3-dihydro-1H-indol-3-yl]-amide

HRID 2040441
ノート
印刷プレビュー

反応式

HRID 2040441 の反応式
C1([O:7][C:8](=O)[NH:9][C:10]2([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[O:28][CH2:29][CH3:30])[C:18]3[C:13](=[CH:14][CH:15]=[C:16]([O:19][CH3:20])[CH:17]=3)[NH:12][C:11]2=[O:21])C=CC=CC=1.[CH3:32][N:33]1[CH2:38][CH2:37][CH:36]([N:39]2[CH2:44][CH2:43][NH:42][CH2:41][CH2:40]2)[CH2:35][CH2:34]1>C1COCC1>[CH2:29]([O:28][C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=1[C:10]1([NH:9][C:8]([N:42]2[CH2:41][CH2:40][N:39]([CH:36]3[CH2:37][CH2:38][N:33]([CH3:32])[CH2:34][CH2:35]3)[CH2:44][CH2:43]2)=[O:7])[C:18]2[C:13](=[CH:14][CH:15]=[C:16]([O:19][CH3:20])[CH:17]=2)[NH:12][C:11]1=[O:21])[CH3:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 5663241-(1-Methyl-4-piperidinyl)piperazineHCID 57517779[3-(2-Ethoxy-phenyl)-5-methoxy-2-oxo-2,3-dihydro-1H-indol-3-yl]-carbamic acid phenyl ester

生成物 1

HCID 575177804-(1-Methyl-piperidin-4-yl)-piperazine-1-carboxylic acid [3-(2-ethoxy-phenyl)-5-methoxy-2-oxo-2,3-dihydro-1H-indol-3-yl]-amide収率 65.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1.9 g (4.5 mmol) of the intermediate from Step D and 1.75 g (9.5 mmol) 1-(1-methylpiperidine-4-yl)-piperazine were dissolved in 30 ml dry THF and refluxed for 90 minutes. The volatiles were removed in vacuo. The resulting residue was dissolved in ethyl acetate, washed with H2O and dried over magnesium sulfate and the solvent was removed in vacuo. The residue was treated with H2O and the resulting precipitate was separated to yield 1.5 g of the intermediate.

後処理

  1. temperaturerefluxed for 90 minutes
  2. customThe volatiles were removed in vacuo
  3. dissolutionThe resulting residue was dissolved in ethyl acetate
  4. washwashed with H2O
  5. dry with materialdried over magnesium sulfate
  6. customthe solvent was removed in vacuo
  7. additionThe residue was treated with H2O
  8. customthe resulting precipitate was separated

出典と根拠

ORDレコード
ord-f20e93a1f2294adfa23c4f3fe5f3d9dd
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08580842B2

反応ノート

読み込み中…

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