Enantholactam → 1-Pent-4-enyl-azocan-2-one

HRID 433069

반응식

HRID 433069 반응식
[H-].[Na+].[NH:3]1[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][C:4]1=[O:11].Br[CH2:13][CH2:14][CH2:15][CH:16]=[CH2:17]>CN(C)C=O>[CH2:17]([N:3]1[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][C:4]1=[O:11])[CH2:16][CH2:15][CH:14]=[CH2:13]

참가 물질

5

반응물 3

HCID 12657EnantholactamHCID 24758Sodium hydrideHCID 707041-Pentene, 5-bromo-

생성물 1

HCID 219785471-Pent-4-enyl-azocan-2-one수율 94.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirred suspension of sodium hydride (0.9 g, 37.5 mmole) in dimethylformamide (50 mL) was added azocan-2-one (3.83 g, 30 mmole). The mixture was stirred at room temperature for 15 minutes, and then 5-bromo-1-pentene (5.03 g, 33.7 mmole) was added slowly. The reaction mixture was stirred at room temperature for 30 minutes, and then at 80° C. for 16 hours. The solvent was removed under reduced pressure and water was added to the residue. The mixture was extracted with ethyl ether, the organic phase was washed with water, dried (magnesium sulfate) and concentrated to give 1-pent-4-enyl-azocan-2-one (5.53 g,) as an oil.

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 30 minutes
  2. waitat 80° C. for 16 hours
  3. customThe solvent was removed under reduced pressure and water
  4. additionwas added to the residue
  5. extractionThe mixture was extracted with ethyl ether
  6. washthe organic phase was washed with water
  7. dry with materialdried (magnesium sulfate)
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5cd3faaf42d842908600841ceb54943e
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06667301B2

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