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

HRID 54551ノート

反応式

HRID 54551 の反応式
[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

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-3fab7586478c4e548ab79ab1c26365a4
出典データセット
uspto-grants-1997_04
特許番号
US05622976

反応ノート

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