Water → HCID 20088003、化合物

HRID 275361ノート

反応式

HRID 275361 の反応式
CO[C:3]([NH:5][CH2:6][CH2:7][N:8]1[CH2:13][CH2:12][CH:11]([N:14]2[C:22]3[C:17](=[CH:18][C:19]([CH3:23])=[CH:20][CH:21]=3)[C:16]([C:24]3[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=3)=[CH:15]2)[CH2:10][CH2:9]1)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[CH3:3][NH:5][CH2:6][CH2:7][N:8]1[CH2:9][CH2:10][CH:11]([N:14]2[C:22]3[C:17](=[CH:18][C:19]([CH3:23])=[CH:20][CH:21]=3)[C:16]([C:24]3[CH:25]=[CH:26][C:27]([F:30])=[CH:28][CH:29]=3)=[CH:15]2)[CH2:12][CH2:13]1

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 20087994HCID 20087994、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 20088003HCID 20088003、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of the crude 1-(1-(N-methoxycarbonyl-2-aminoethyl)-4-piperidyl)-3-(4-fluorophenyl)-5-methyl-1H-indole (8.8 g) in dry tetrahydrofuran (75 ml) was added to a suspension of lithium aluminum hydride (2 g) in dry tetrahydrofuran (75 ml) during 15 min and the reaction mixture was refluxed for 1.5 h. After cooling on an ice bath water (4 ml), 4N aqueous NaOH (2.5 ml) and water (10 ml) were added, succesively. The precipitate was filtered off, the solution was dried (Na2SO4) and the solvents were evaporated. This afforded the title compound, as an oil Yield: 6.9 g.

後処理

  1. temperaturethe reaction mixture was refluxed for 1.5 h
  2. additionwere added
  3. filtrationThe precipitate was filtered off
  4. dry with materialthe solution was dried (Na2SO4)
  5. customthe solvents were evaporated

出典と根拠

ORDレコード
ord-581ac795692a40c58a0527e9f021a5a6
出典データセット
uspto-grants-1995_02
特許番号
US05393761

反応ノート

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