1,1-Dicyclopropyl-2-dibenzylamino-ethanol → 2-Amino-1,1-dicyclopropylethan-1-ol

HRID 1865893ノート

反応式

HRID 1865893 の反応式
[CH:1]1([C:4]([CH:22]2[CH2:24][CH2:23]2)([OH:21])[CH2:5][N:6](CC2C=CC=CC=2)CC2C=CC=CC=2)[CH2:3][CH2:2]1.[H][H]>CO.[OH-].[OH-].[Pd+2].C>[NH2:6][CH2:5][C:4]([CH:22]1[CH2:24][CH2:23]1)([CH:1]1[CH2:3][CH2:2]1)[OH:21]

参加物

5

反応物 2

HCID 687982851,1-Dicyclopropyl-2-dibenzylamino-ethanolHCID 178418361HCID 178418361、化合物

生成物 1

HCID 552845292-Amino-1,1-dicyclopropylethan-1-ol収率 81.4%

試薬・触媒・溶媒 2

HCID 86583698HCID 86583698、化合物触媒HCID 887Methanol溶媒

実験手順

To a solution of 0.28 g 1,1-dicyclopropyl-2-dibenzylamino-ethanol (0.00087 mol) in 10 ml methanol was added 0.060 g Pd(OH)2/charcoal (Fluka 7663; 20%) and the mixture was hydrogenated under 8 bar hydrogen pressure at 60° C. for 2 hours. The catalyst was removed by filtration and the mother liquor was concentrated and the residue was purified by chromatography on silicagel with MeCl2/MeOH/NH3 90:10:1 to yield 0.10 g (81% yield) of the title compound as colorless oil. 1H-NMR (CDCl3 300 MHz, δ ppm) 0.28-0.45 (m, 8H); 0.71-0.78 (m, 2H); 2.77 (s, 2H) ppm.

後処理

  1. customThe catalyst was removed by filtration
  2. concentrationthe mother liquor was concentrated
  3. customthe residue was purified by chromatography on silicagel with MeCl2/MeOH/NH3 90:10:1

出典と根拠

ORDレコード
ord-5338c02ab66f43eab5e494373880c204
出典データセット
uspto-grants-2009_12
特許番号
US07629346B2

反応ノート

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