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3-(Benzyl-methyl-amino)-butyric acid methyl ester → Methyl 3-(methylamino)butanoate

HRID 480248
ノート
印刷プレビュー

反応式

HRID 480248 の反応式
[CH3:1][O:2][C:3](=[O:16])[CH2:4][CH:5]([N:7](CC1C=CC=CC=1)[CH3:8])[CH3:6]>CO.[OH-].[OH-].[Pd+2]>[CH3:1][O:2][C:3](=[O:16])[CH2:4][CH:5]([NH:7][CH3:8])[CH3:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 232160883-(Benzyl-methyl-amino)-butyric acid methyl ester

生成物 1

HCID 12636115Methyl 3-(methylamino)butanoate

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 887Methanol溶媒2 回

実験手順

3-(Benzyl-methyl-amino)-butyric acid methyl ester (15 g, 67.8 mmol, 1.0 equiv) was placed in a Parr hydrogenation bottle and dissolved in 50 mL of MeOH. 20% Palladium hydroxide on carbon (0.5 g, 0.94 mmol, 0.014 equiv) was added and the mixture was shaken at 50 psi H2 for 16 h. The reaction was judged as complete when the uptake of H2 had stopped. The bottle was opened and 10 g of diatomaceous earth in 100 mL of MeOH was added. The mixture was filtered on a pad of diatomaceous earth which was then washed with 2×100 mL of MeOH. The filtrates were combined and concentrated in vacuo to yield the desired product as an oil that is somewhat volatile (7.6 g, 85%). The crude product was used without further purification; MS, m/z 132=M+1.

後処理

  1. filtrationThe mixture was filtered on a pad of diatomaceous earth which
  2. washwas then washed with 2×100 mL of MeOH
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-95867b2c82474370a76bd2b91692c3a7
出典データセット
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06649642B2

反応ノート

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