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2-Methylimidazole → 3-(2-(2-Methyl-1H-imidazol-1-YL)acetyl)benzonitrile

HRID 2214765
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HRID 2214765 반응식
[C:1]([C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[C:7]#[N:8])(=[O:3])[CH3:2].BrBr.[CH3:14][C:15]1[NH:16][CH:17]=[CH:18][N:19]=1>O1CCOCC1.C(#N)C>[CH3:14][C:15]1[N:16]([CH2:2][C:1]([C:4]2[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=2)[C:7]#[N:8])=[O:3])[CH:17]=[CH:18][N:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 127492-MethylimidazoleHCID 24408BromineHCID 802223-Acetylbenzonitrile

생성물 1

HCID 219484043-(2-(2-Methyl-1H-imidazol-1-YL)acetyl)benzonitrile

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 312751,4-Dioxane용매

실험 절차

3-acetylbenzonitrile (50 g, 0.345 mol) is dissolved in dioxane (600 ml) with stirring at room temperature, bromine (17.7 ml, 0.345 mol) is added in and the mixture is stirred for 30 minutes. The dioxane is removed in vacuo to give a solid which is dissolved in acetonitrile (300 ml). 2-Methylimidazole (28.3 g, 0.345 mol) is added to the solution and the mixture is stirred for 1 hour, the temperature of the mixture rising to 45° C. The precipated solid is filtered off, washed with acetonitrile, and slurried with methanol for 1 hour. After filtering to remove undissolved solid, the filtrate is evaporated in vacuo to leave a solid which is dried in vacuo at 40° C. to give the title compound, m.s. 369 (MH+).

후처리

  1. stirringis stirred for 30 minutes
  2. customThe dioxane is removed in vacuo
  3. customto give a solid which
  4. stirringthe mixture is stirred for 1 hour
  5. customrising to 45° C
  6. filtrationThe precipated solid is filtered off
  7. washwashed with acetonitrile
  8. filtrationAfter filtering
  9. customto remove undissolved solid
  10. customthe filtrate is evaporated in vacuo
  11. customto leave a solid which
  12. customis dried in vacuo at 40° C.

출처 및 근거

ORD 기록
ord-ee23e65dbae84229a0ef69d6c43a6777
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07109202B2

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