4-Methyl-3-oxo-1-(phenylmethyl)proline ethyl ester → 1-Benzyl-4-methylpyrrolidin-3-one

HRID 846695ノート

反応式

HRID 846695 の反応式
C(OC([CH:6]1[C:10](=[O:11])[CH:9]([CH3:12])[CH2:8][N:7]1[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=O)C>Cl>[CH2:13]([N:7]1[CH2:8][CH:9]([CH3:12])[C:10](=[O:11])[CH2:6]1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

参加物

3

反応物 1

HCID 545049354-Methyl-3-oxo-1-(phenylmethyl)proline ethyl ester

生成物 1

HCID 124309801-Benzyl-4-methylpyrrolidin-3-one

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
100 °C

実験手順

A 30.15 g (115.4 mmol) sample of the ester from step c was hydrolyzed and decarboxylated by adding to 280 mL of 1M HCl and heating at 100° C. under reflux conditions for 12 hours. The mixture was then poured over ice and the impurities extracted into methylene chloride. The aqueous solution was then adjusted to pH 8 with potassium carbonate and the product extracted into methylene chloride, which was then dried over anhydrous sodium sulfate. The solvent was removed by evaporation under vacuum, to yield 9.95 g of 1-benzyl-4-methylpyrrolidin-3-one, NMR (CDCl3) d 1.12 (d, 3H, J=7.5 Hz), 2.50 (m, 1H), 2.75 (m, 2H), 3.33 (m, 2H), 3.69 (d, 2H, J=7.5 Hz), 7.32 (m, 5H).

後処理

  1. additionThe mixture was then poured over ice
  2. extractionthe impurities extracted into methylene chloride
  3. extractionthe product extracted into methylene chloride, which
  4. dry with materialwas then dried over anhydrous sodium sulfate
  5. customThe solvent was removed by evaporation under vacuum

出典と根拠

ORDレコード
ord-cc6d2c82379645ea91639be810597d74
出典データセット
uspto-grants-1992_08
特許番号
US05137892

反応ノート

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