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

HRID 846695노트

반응식

HRID 846695 반응식
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

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
100 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-cc6d2c82379645ea91639be810597d74
출처 데이터셋
uspto-grants-1992_08
특허 번호
US05137892

반응 노트

불러오는 중…