Hydrochloric Acid → 2-Methyl-2-(1-methylpiperidin-3-yl)propanoic acid

HRID 2237748ノート

反応式

HRID 2237748 の反応式
C[O:2][C:3](=[O:14])[C:4]([CH3:13])([CH:6]1[CH2:11][CH2:10][CH2:9][N:8]([CH3:12])[CH2:7]1)[CH3:5].[OH-].[Li+].Cl>CO>[CH3:13][C:4]([CH:6]1[CH2:11][CH2:10][CH2:9][N:8]([CH3:12])[CH2:7]1)([CH3:5])[C:3]([OH:14])=[O:2]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 668891612-Methyl-2-(1-methyl-piperidin-3(r,s)-yl)-propionic acid methyl ester

生成物 1

HCID 668879152-Methyl-2-(1-methylpiperidin-3-yl)propanoic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

0.200 g of 2-methyl-2-(1-methyl-piperidin-3(R,S)-yl)-propionic acid methyl ester are dissolved in 4 ml of methanol. 4 ml of a 1M aqueous lithium hydroxide solution are added and the mixture is stirred for 16 hours at room temperature. The reaction mixture is neutralised with 1M HCl and extracted with ethyl acetate (3×50 ml). The organic phases are combined and concentrated by evaporation. The residue is purified by means of flash chromatography (SiO2 60F) to provide the title compound as a colourless oil. Rf 0.15 (150:54:10:1 dichloromethane-methanol-acetic acid-water).

後処理

  1. extractionextracted with ethyl acetate (3×50 ml)
  2. concentrationconcentrated by evaporation
  3. customThe residue is purified by means of flash chromatography (SiO2 60F)

出典と根拠

ORDレコード
ord-60558e219e82451e913faedc4e4ade57
出典データセット
uspto-grants-2010_05
特許番号
US07718675B2

反応ノート

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