3-Oxocyclobutane-1-carbonitrile → 3-(2-(5-Bromo-2-methoxypyridin-3-yl)-2-oxoethylidene)cyclobutanecarbonitrile

HRID 473363노트

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HRID 473363 반응식
[Br:1][C:2]1[CH:3]=[C:4](/[C:10](/[O-:18])=[CH:11]/P(OC)(OC)=O)[C:5]([O:8][CH3:9])=[N:6][CH:7]=1.[Li+].O=[C:21]1[CH2:24][CH:23]([C:25]#[N:26])[CH2:22]1>O1CCOCC1.O>[Br:1][C:2]1[CH:3]=[C:4]([C:10](=[O:18])[CH:11]=[C:21]2[CH2:24][CH:23]([C:25]#[N:26])[CH2:22]2)[C:5]([O:8][CH3:9])=[N:6][CH:7]=1

참가 물질

5

반응물 2

HCID 130823903-Oxocyclobutane-1-carbonitrileHCID 59468662lithium (Z)-1-(5-bromo-2-methoxypyridin-3-yl)-2-(dimethoxyphosphoryl)ethenolate

생성물 1

HCID 575158633-(2-(5-Bromo-2-methoxypyridin-3-yl)-2-oxoethylidene)cyclobutanecarbonitrile

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

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온도
120 °C

실험 절차

A mixture of lithium (Z)-1-(5-bromo-2-methoxypyridin-3-yl)-2-(dimethoxyphosphoryl)ethenolate (2.0 g, 5.8 mmol) and 3-oxocyclobutanecarbonitrile (1.1 g, 12 mmol) in p-dioxane (6 ml) was heated at 120° C. by Microwave in 1 h. The mixture was cooled, taken up in H2O, extracted with EtOAc (3×), dried over MgSO4, concentrated to provide the title compound. MS (m+11): 307.0.

후처리

  1. temperatureThe mixture was cooled
  2. extractionextracted with EtOAc (3×)
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f4f3713c570341ffb0c4fb1f1e1907ee
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08633315B2

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