Ethanol → 1-Allyl-6-ethoxy-4-methylhexahydropyrimidin-2-one

HRID 1607381

반응식

HRID 1607381 반응식
[CH2:1]([NH:4][C:5]([NH2:7])=[O:6])[CH:2]=[CH2:3].[CH:8](=[O:12])/[CH:9]=[CH:10]/[CH3:11].[CH3:13][CH2:14]O>Cl>[CH2:1]([N:4]1[CH:8]([O:12][CH2:13][CH3:14])[CH2:9][CH:10]([CH3:11])[NH:7][C:5]1=[O:6])[CH:2]=[CH2:3]

참가 물질

5

반응물 3

HCID 702EthanolHCID 11181AllylureaHCID 447466Crotonaldehyde2회

생성물 1

HCID 193761321-Allyl-6-ethoxy-4-methylhexahydropyrimidin-2-one

시약·촉매·용매 1

HCID 313Hydrochloric Acid촉매

실험 절차

Following a related procedure, [G. Zigeuner, W. Rauter, Monatshefte fur Chemie, 96, 1950 (1965)], allylurea (24.5 g, 0.25 mol), crotonaldehyde (19.67 g, 0.29 mol) and 37% HCl (12 drops) were mixed with 140 g of EtOH at room temperature for 3d, during which all of the crotonaldehyde was consumed. The major product had a retention time near that of allylurea. The dark mixture was neutralized with Na2CO3, filtered and concentrated at reduced pressure. Part of the crude mixture was extracted with cyclohexane, decolorized with charcoal, filtered and concentrated to give a light yellow oil which produced white crystals (mp 72°-76° C.) on standing. A separate sample was submitted to kugelrohr distillation (0.05 torr) to give further products: E at 90° C., F at 145°-155° C. (solid, mp 72°-76° C.) and G at 145°-155° C. (liquid).

후처리

  1. customwas consumed
  2. filtrationfiltered
  3. concentrationconcentrated at reduced pressure
  4. extractionPart of the crude mixture was extracted with cyclohexane
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto give a light yellow oil which

출처 및 근거

ORD 기록
ord-ec717c1fb8ff42f0bad35b17e9488a59
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04864055

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