Water → (R)-(1-methylpiperidin-3-yl)methanol

HRID 454002

反応式

HRID 454002 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][CH2:5][C@@H:4]([C:8](OCC)=[O:9])[CH2:3]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>CCOCC.C1COCC1>[CH3:1][N:2]1[CH2:7][CH2:6][CH2:5][C@@H:4]([CH2:8][OH:9])[CH2:3]1

参加物

7

反応条件

温度
20 °C

実験手順

A solution of (R)-ethyl 1-methylpiperidine-3-carboxylate (5.69 g, 33 mmol) in ether (20 ml) was added dropwise to a stirred solution of lithium aluminium hydride (36.6 ml of a 1M solution in THF, 36.6 mmol) in ether (85 ml) cooled to maintain a reaction temperature of 20° C. The mixture was stirred for 1.5 hours at ambient temperature and then water (1.4 ml), 15% aqueous sodium hydroxide solution (1.4 ml) and then water (4.3 ml) were added. The insolubles were removed by filtration and the volatiles removed from the filtrate by evaporation to give (R)-(1-methylpiperidin-3-yl)methanol (4.02 g, 94%) as a colourless oil.

後処理

  1. temperaturecooled
  2. customThe insolubles were removed by filtration
  3. customthe volatiles removed from the filtrate by evaporation

出典と根拠

ORDレコード
ord-1e40f4b3c64b468296342a4fc7788663
出典データセット
uspto-grants-2013_07
特許番号
US08492560B2

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