1-[1-(4-Bromophenyl)-butyl]-imidazole → 4-[1-(1-Imidazolyl)-butyl]-benzonitrile

HRID 727845노트

반응식

HRID 727845 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([CH:8]([N:12]2[CH:16]=[CH:15][N:14]=[CH:13]2)[CH2:9][CH2:10][CH3:11])=[CH:4][CH:3]=1.[Cu][C:18]#[N:19]>CN1CCCC1>[N:12]1([CH:8]([C:5]2[CH:6]=[CH:7][C:2]([C:18]#[N:19])=[CH:3][CH:4]=2)[CH2:9][CH2:10][CH3:11])[CH:16]=[CH:15][N:14]=[CH:13]1

참가 물질

4

반응물 2

HCID 145143611-[1-(4-Bromophenyl)-butyl]-imidazoleHCID 178418546HCID 178418546, 화합물

생성물 1

HCID 145143624-[1-(1-Imidazolyl)-butyl]-benzonitrile수율 68.4%

시약·촉매·용매 1

HCID 84541-Methylpyrrolidine용매

실험 절차

2.79 g of 1-[1-(4-bromophenyl)-butyl]-imidazole and 1.8 g of copper(I) cyanide are heated in 5 ml of N-methylpyrrolidine for 4 hours at 180° C. under a protecting gas atmosphere (argon). After cooling, it is precipitated in 50 ml of ammonia solution, stirred for 15 more minutes at room temperature and extracted with ethyl acetate. After concentration by evaporation in a vacuum 1.95 g of dark oil is obtained. This oil is distilled on a bulb tube in a vacuum; boiling point 200°-215° C./0.05 mbar. The resulting distillate is recrystallized from ethanol/petroleum ether. 1.54 g of 4-[1-(1-imidazolyl)-butyl]-benzonitrile with a melting point of 63°-71° C. is obtained.

후처리

  1. temperatureAfter cooling
  2. customit is precipitated in 50 ml of ammonia solution
  3. extractionextracted with ethyl acetate
  4. concentrationAfter concentration
  5. customby evaporation in a vacuum 1.95 g of dark oil
  6. customis obtained
  7. distillationThis oil is distilled on a bulb tube in a vacuum
  8. customThe resulting distillate is recrystallized from ethanol/petroleum ether

출처 및 근거

ORD 기록
ord-39a1a68327464ac18d2e006432f27dd7
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05045558

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