Sodium Hydroxide → 2-[1-(3-Methoxybenzyl)piperidin-4-yl]ethylamine

HRID 54551노트

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HRID 54551 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:17]=[CH:18][CH:19]=1)[C:6]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][CH2:15][NH2:16])[CH2:10][CH2:9]1)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+].S([O-])([O-])(=O)=O.[Mg+2]>O1CCCC1.O.C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:17]=[CH:18][CH:19]=1)[CH2:6][N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][CH2:15][NH2:16])[CH2:10][CH2:9]1

참가 물질

8

반응물 4

HCID 14798Sodium HydroxideHCID 24083Sulfuric acid magnesium salt (1:1)HCID 199591472-[1-(3-Methoxybenzoyl)piperidin-4-yl]ethylamineHCID 21226445Aluminium lithium hydride

생성물 1

HCID 199591902-[1-(3-Methoxybenzyl)piperidin-4-yl]ethylamine수율 42.3%

시약·촉매·용매 3

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

A solution of 2-[1-(3-methoxybenzoyl)piperidin-4-yl]ethylamine (4.5 g) in tetrahydrofuran (40 ml) was added dropwise to a suspension of lithium aluminum hydride (1.63 g) in tetrahydrofuran (50 ml) under refluxing. After 30 minutes, the mixture was cooled to 0° C., and ethyl acetate (5 ml), water (2 ml), 4N sodium hydroxide (4 ml), water (2 ml) and magnesium sulfate were added thereto successively. The resulting precipitates were removed out by filtration and the filtrate was evaporated in vacuo. The residue was chromagographed on alumina eluting with 2% methanol in chloroform to give 2-[1-(3-methoxybenzyl)piperidin-4-yl]ethylamine (1.8 g) as an oil.

후처리

  1. temperatureunder refluxing
  2. customThe resulting precipitates
  3. customwere removed out by filtration
  4. customthe filtrate was evaporated in vacuo

출처 및 근거

ORD 기록
ord-3fab7586478c4e548ab79ab1c26365a4
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05622976

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