3-(Trifluoromethyl)phenylcyanamide → HCID 178490592, 화합물

HRID 636684

반응식

HRID 636684 반응식
[NH:1]([C:4]1[CH:5]=[C:6]([C:10]([F:13])([F:12])[F:11])[CH:7]=[CH:8][CH:9]=1)[C:2]#[N:3].Cl.[CH3:15][O:16][C:17]1[CH:23]=[CH:22][C:21]([C:24]([F:27])([F:26])[F:25])=[CH:20][C:18]=1[NH2:19]>C(#N)C>[CH3:15][O:16][C:17]1[CH:23]=[CH:22][C:21]([C:24]([F:25])([F:26])[F:27])=[CH:20][C:18]=1[NH:19][C:2]([NH:1][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]([F:11])([F:12])[F:13])[CH:5]=1)=[NH:3]

참가 물질

4

반응물 2

HCID 110741023-(Trifluoromethyl)phenylcyanamideHCID 700096092-Methoxy-5-(trifluoromethyl)aniline hydrochloride

생성물 1

HCID 178490592HCID 178490592, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 3-cyanamidobenzotrifluoride (0.40 g, 2.15 mmol), 2-methoxy-5-triflouromethylaniline hydrochloric acid salt (0.53 g, 2.33 mmol) and acetonitrile (20 ml) was stirred at reflux for 40 h. The solvent was evaporated. Dichloromethane (50 ml) was added and the mixture was washed with saturated aqueous sodium hydrogen carbonate (50 ml). The organic phase was purified by chromatography using silica gel and a mixture of methanol (10%) and dichloromethane as eluent. The product was isolated as the free base. Yield 0.40 g, 49%. M.p. 45-47° C.

후처리

  1. temperatureat reflux for 40 h
  2. customThe solvent was evaporated
  3. additionDichloromethane (50 ml) was added
  4. washthe mixture was washed with saturated aqueous sodium hydrogen carbonate (50 ml)
  5. customThe organic phase was purified by chromatography
  6. additiona mixture of methanol (10%) and dichloromethane as eluent
  7. customThe product was isolated as the free base

출처 및 근거

ORD 기록
ord-8d904f464e7541fe803fbfa70b6cc7c7
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06194447B1

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