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Water → 3-[3-(4-methylpiperazin-1-yl)propyl]-4,5,6,7-tetrahydro-1H-indole

HRID 24339
ノート
印刷プレビュー

反応式

HRID 24339 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[CH3:7][N:8]1[CH2:13][CH2:12][N:11]([C:14](=O)[CH2:15][CH2:16][C:17]2[C:25]3[C:24](=O)[CH2:23][CH2:22][CH2:21][C:20]=3[NH:19][CH:18]=2)[CH2:10][CH2:9]1.O>C1COCC1.[OH-].[Na+]>[CH3:7][N:8]1[CH2:9][CH2:10][N:11]([CH2:14][CH2:15][CH2:16][C:17]2[C:25]3[CH2:24][CH2:23][CH2:22][CH2:21][C:20]=3[NH:19][CH:18]=2)[CH2:12][CH2:13]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 225710693-[3-(4-Methylpiperazin-1-yl)-3-oxo-propyl]-1,5,6,7-tetrahydroindol-4-one

生成物 1

HCID 225711153-[3-(4-methylpiperazin-1-yl)propyl]-4,5,6,7-tetrahydro-1H-indole収率 101.3%

試薬・触媒・溶媒 2

HCID 14798Sodium Hydroxide触媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

LAH (2.6 g, 68 mmol) was added dropwise to a suspension of 3-[3-(4-methylpiperazin-1-yl)-3-oxo-propyl]-1,5,6,7-tetrahydroindol-4-one (5 g, 17 mmol) in THF (300 mL). The mixture was then refluxed overnight. The mixture was then cooled and 2.6 mL each of water followed by a few drops of 15% NaOH was added. The reaction was stirred at room temperature for 30 min and then filtered to remove insolubles. The filtrate was concentrated to give 4.5 g (100%) of 3-[3-(4-methylpiperazin-1-yl)propyl]-4,5,6,7-tetrahydro-1H-indole.

後処理

  1. temperatureThe mixture was then refluxed overnight
  2. temperatureThe mixture was then cooled
  3. additionwas added
  4. filtrationfiltered
  5. customto remove insolubles
  6. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-8aef07f7b52743baa5ff07de3736c246
出典データセット
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06855730B2

反応ノート

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