Allyl Alcohol → HCID 18617566、化合物

HRID 1264312ノート

反応式

HRID 1264312 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 18617566HCID 18617566、化合物

試薬・触媒・溶媒 1

HCID 11026Titanium isopropoxide触媒2 回

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-62f61683d4c54a9d8b9daa72a035e847
出典データセット
uspto-grants-2003_04
特許番号
US06541505B1

反応ノート

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