Sodium Sulfate → 5-(4-Nitrophenyl)-2-(trifluoromethyl)-1H-imidazole

HRID 56603

반응식

HRID 56603 반응식
[F:1][C:2]([F:7])([F:6])[C:3](=[NH:5])[NH2:4].Br[CH2:9][C:10]([C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=1)=O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C(#N)C>[N+:18]([C:15]1[CH:16]=[CH:17][C:12]([C:10]2[NH:4][C:3]([C:2]([F:7])([F:6])[F:1])=[N:5][CH:9]=2)=[CH:13][CH:14]=1)([O-:20])=[O:19]

참가 물질

5

반응물 3

HCID 24436Sodium SulfateHCID 668402-Bromo-4'-nitroacetophenoneHCID 2776882Trifluoroacetamidine

생성물 1

HCID 1176226405-(4-Nitrophenyl)-2-(trifluoromethyl)-1H-imidazole

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

324 mg (purity 85%, 2.5 mmol, 3 eq.) of 2,2,2-trifluoroethaneimidamide were added to a suspension of 200 mg (0.82 mmol) of 2-bromo-1-(4-nitrophenyl)ethanone and 500 mg of sodium sulphate in 10 ml of acetonitrile, and the mixture was treated in an ultrasonic bath for 1 h and then stirred at RT. The sodium sulphate was then filtered off and the filtrate was concentrated under reduced pressure. The residue was purified by preparative HPLC (Reprosil C18, water/methanol gradient). Yield: 104 mg (49% of theory)

후처리

  1. additionthe mixture was treated in an ultrasonic bath for 1 h
  2. filtrationThe sodium sulphate was then filtered off
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by preparative HPLC (Reprosil C18, water/methanol gradient)

출처 및 근거

ORD 기록
ord-5cf9c54dfb5748f79e911f130afe5c05
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434690B2

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