Water → 4-(2-(2,6-Dimethyl-3-nitrophenoxy)pyridin-3-yl)pyrimidine

HRID 1361686

반응식

HRID 1361686 반응식
[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4]([CH3:11])[C:3]=1[OH:12].Cl[C:14]1[C:19]([C:20]2[CH:25]=[CH:24][N:23]=[CH:22][N:21]=2)=[CH:18][CH:17]=[CH:16][N:15]=1.C(=O)([O-])[O-].[Cs+].[Cs+].O>CS(C)=O>[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4]([CH3:11])[C:3]=1[O:12][C:14]1[C:19]([C:20]2[CH:25]=[CH:24][N:23]=[CH:22][N:21]=2)=[CH:18][CH:17]=[CH:16][N:15]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 10796Cesium carbonateHCID 814763-Nitro-2,6-xylenolHCID 161089744-(2-Chloropyridin-3-yl)pyrimidine

생성물 1

HCID 669706854-(2-(2,6-Dimethyl-3-nitrophenoxy)pyridin-3-yl)pyrimidine

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

Dissolved 2,6-dimethyl-3-nitrophenol (1.96 g, 11.7 mmol) and 4-(2-chloropyridin-3-yl)pyrimidine (1.50 g, 7.83 mmol) in dimethylsulfoxide (15.0 ml) and added cesium carbonate (5.10 g, 15.7 mmol). Reaction mixture was heated to 1200C in a sealed tube for 8 hours. Reaction mixture was then allowed to cool to room temperature and then poured into 250 mL of rapidly stirring water in an Erlenmeyer flask. After 10 minutes, the opaque brown aqueous solution was cooled to 0° C. and allowed to stand for 10 minutes, then filtered. The precipitate was collected as the title compound. MS m/z=323 (M+H)+. Calc'd for C17H16N4O3: 324.34.

후처리

  1. customReaction mixture
  2. customReaction mixture
  3. temperaturethe opaque brown aqueous solution was cooled to 0° C.
  4. waitto stand for 10 minutes
  5. filtrationfiltered
  6. customThe precipitate was collected as the title compound

출처 및 근거

ORD 기록
ord-9896c3dafcf04df5a1785cc19e976847
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07880000B2

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