Allyl Alcohol → HCID 18617566, 화합물

HRID 1264312노트

반응식

HRID 1264312 반응식
[O:1]=[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:18]=[CH:17][C:11]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:10][CH:9]=2)=[CH:4][NH:3]1.[CH2:19](O)C=C>CC(C)[O-].[Ti+4].CC(C)[O-].CC(C)[O-].CC(C)[O-]>[O:1]=[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:18]=[CH:17][C:11]([C:12]([O:14][CH2:15][CH:16]=[CH2:19])=[O:13])=[CH:10][CH:9]=2)=[CH:4][NH:3]1

참가 물질

4

반응물 2

HCID 7858Allyl AlcoholHCID 18617564Ethyl 4-(6-oxo-1,6-dihydropyridin-3-yl)benzoate

생성물 1

HCID 18617566HCID 18617566, 화합물

시약·촉매·용매 1

HCID 11026Titanium isopropoxide촉매2회

실험 절차

To a solution of ethyl 4-(2-oxo-2H-pyridin-5-yl)benzoate (1.24 g, 5.10 mmoles, reference example 36f) in allyl alcohol (50 mL) was added titanium (IV) isopropoxide. The resulting mixture was heated to 70° C. for seven hours at which point more titanium (IV) isopropoxide (3 mL) was added. After 18 hours the heat was removed and 1N HCl solution (50 mL) was added followed by extraction with CH2Cl2 (200 mL). The organic layer was isolated and concentrated to give the title compound in quantitative yield. MS (ion spray) m/z 256 (M+H)+.

후처리

  1. additionwas added
  2. customAfter 18 hours the heat was removed
  3. addition1N HCl solution (50 mL) was added
  4. extractionfollowed by extraction with CH2Cl2 (200 mL)
  5. customThe organic layer was isolated
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-62f61683d4c54a9d8b9daa72a035e847
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06541505B1

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