Ethyl Acetoacetate → 3-Allyl-6-methyluracil

HRID 349288

반응식

HRID 349288 반응식
[CH2:1]([NH:4][C:5]([NH2:7])=[O:6])[CH:2]=[CH2:3].[C:8](OCC)(=[O:13])[CH2:9][C:10]([CH3:12])=O.[OH-].[K+]>C(O)C.Cl.CO>[CH2:1]([N:4]1[C:8](=[O:13])[CH:9]=[C:10]([CH3:12])[NH:7][C:5]1=[O:6])[CH:2]=[CH2:3]

참가 물질

7

반응물 3

HCID 8868Ethyl AcetoacetateHCID 11181AllylureaHCID 14797Potassium Hydroxide

생성물 1

HCID 136020473-Allyl-6-methyluracil

시약·촉매·용매 3

HCID 313Hydrochloric Acid촉매HCID 702Ethanol용매HCID 887Methanol용매

실험 절차

To allylurea (25 g, 0.25 mol) in ethanol (10 mL) was added ethyl acetoacetate (31.86 mL, 0.25 mol) and 10 drops conc. HCl. After 12 days at room temperature, concentration gave an oil which was dissolved in MeOH. KOH (22.5 g, 0.34 mol) was added and the solution refluxed for 1 hour. After neutralization, the resulting solid 1 was collected. Yield 2.7 g (7%). NMR (CDCl3) δ: 2.16 (3H, s), 4.52 (2H, d), 5.18 (1H, d), 5.23 (1H, d), 5.60 (1H, s), 5.82–5.93 (1H, m), 10.3 (1H, s).

후처리

  1. concentrationconcentration
  2. customgave an oil which
  3. temperaturethe solution refluxed for 1 hour
  4. customAfter neutralization, the resulting solid 1 was collected

출처 및 근거

ORD 기록
ord-07db849e044840039386e1356153d402
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179815B2

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