Water → HCID 20088003, 화합물

HRID 275361노트

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HRID 275361 반응식
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

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 20087994HCID 20087994, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 20088003HCID 20088003, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-581ac795692a40c58a0527e9f021a5a6
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05393761

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