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 546882노트

반응식

HRID 546882 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-8508f2ddddb94deb899cc4ae3deafdac
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07935688B2

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