2,2-Dimethyl-1,3-dioxane-4,6-dione → 5-(5-Bromopyridin-2(1H)-ylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione

HRID 546882ノート

反応式

HRID 546882 の反応式
[CH3:1][C:2]1([CH3:10])[O:9][C:7](=[O:8])[CH2:6][C:4](=[O:5])[O:3]1.[Br:11][C:12]1[CH:13]=[N+:14]([O-])[CH:15]=[CH:16][CH:17]=1>C(OC(=O)C)(=O)C>[Br:11][C:12]1[CH:17]=[CH:16][C:15](=[C:6]2[C:7](=[O:8])[O:9][C:2]([CH3:10])([CH3:1])[O:3][C:4]2=[O:5])[NH:14][CH:13]=1

参加物

4

反応物 2

HCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 142763Pyridine, 3-bromo-, 1-oxide

生成物 1

HCID 574434985-(5-Bromopyridin-2(1H)-ylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione収率 33%

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

実験手順

Meldrum's acid (6.63 g, 45.98 mmol) was added to a solution of 3-bromopyridine N-oxide (8 g, 45.98 mmol) in acetic anhydride (50 mL), and the mixture was stirred at room temperature overnight. Then, the reaction mixture was concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (hexane:ethyl acetate and ethyl acetate) to give the target compound (4.53 g, 33%).

後処理

  1. concentrationThen, the reaction mixture was concentrated under reduced pressure
  2. customThe resulting residue was purified by silica gel chromatography (hexane:ethyl acetate and ethyl acetate)

出典と根拠

ORDレコード
ord-8508f2ddddb94deb899cc4ae3deafdac
出典データセット
uspto-grants-2011_05
特許番号
US07935688B2

反応ノート

読み込み中…