Methyl iodide → 5-(4-Methylbenzylidene)-3-(2,5-difluorophenyl)-1-methylimidazolidine-2,4-dione

HRID 1165693노트

반응식

HRID 1165693 반응식
[CH3:1][C:2]1[CH:23]=[CH:22][C:5]([CH:6]=[C:7]2[NH:11][C:10](=[O:12])[N:9]([C:13]3[CH:18]=[C:17]([F:19])[CH:16]=[CH:15][C:14]=3[F:20])[C:8]2=[O:21])=[CH:4][CH:3]=1.[C:24](=O)([O-])[O-].[Cs+].[Cs+].CI>CN(C=O)C.O>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([CH:6]=[C:7]2[N:11]([CH3:24])[C:10](=[O:12])[N:9]([C:13]3[CH:18]=[C:17]([F:19])[CH:16]=[CH:15][C:14]=3[F:20])[C:8]2=[O:21])=[CH:22][CH:23]=1

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 54007378HCID 54007378, 화합물

생성물 1

HCID 537367675-(4-Methylbenzylidene)-3-(2,5-difluorophenyl)-1-methylimidazolidine-2,4-dione수율 186.3%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

The 5-(4-methylbenzylidene)-3-(2,5-difluorophenyl)imidazolidine-2,4-dione (2.25 g, 7.16 mmol), cesium carbonate (1.22 g, 3.76 mmol) and methyl iodide (1.5 g, 3.76 mmol) were stirred together in DMF (20 mL) overnight. The solution was then diluted with water and extracted with ethyl acetate (3×). The combined extracts were washed with brine (saturated), dried (over MgSO4), filtered and concentrated to give 2.3 grams of 5-(4-methylbenzylidene)-3-(2,5-difluorophenyl)-1-methylimidazolidine-2,4-dione, m.p. 136°-140° C. (compound 104 under Table B).

후처리

  1. extractionextracted with ethyl acetate (3×)
  2. washThe combined extracts were washed with brine (saturated)
  3. dry with materialdried (over MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1d0f4f3c74cb40cd8079abffbee4e705
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04911748

반응 노트

불러오는 중…