Water → 2-[3-(Trifluoromethyl)phenyl]propanenitrile

HRID 660888노트

반응식

HRID 660888 반응식
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:4]=[C:5]([CH2:9][C:10]#[N:11])[CH:6]=[CH:7][CH:8]=1.I[CH3:15].[NH2-].[Na+].O>C1(C)C=CC=CC=1.ClCCl>[F:1][C:2]([F:12])([F:13])[C:3]1[CH:4]=[C:5]([CH:9]([CH3:15])[C:10]#[N:11])[CH:6]=[CH:7][CH:8]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24533Sodium amideHCID 75360m-Trifluoromethylphenylacetonitrile

생성물 1

HCID 108456762-[3-(Trifluoromethyl)phenyl]propanenitrile

시약·촉매·용매 2

HCID 1140Toluene용매2회HCID 6344Dichloromethane용매

반응 조건

온도
80 °C

실험 절차

1.0 g (5.4 mmol) of 3-(trifluoromethyl)phenylacetonitrile and 767 mg of iodomethane (5.4 mmol) are placed in 5 ml toluene at 80° C. and slowly treated with a 50% suspension of sodamide in toluene. Next the mixture is stirred 1 hr more at 80° C., then cooled to RT and treated with water, then dichloromethane. The organic phase is separated, washed with water, dried over magnesium sulphate and freed of solvent on the rotary evaporator. The residue (1.7 g, 84% of theory) contains the title compound with a purity of ca. 53% by GC/MS and is used without purification for the next reaction.

후처리

  1. temperaturecooled to RT
  2. customThe organic phase is separated
  3. washwashed with water
  4. dry with materialdried over magnesium sulphate
  5. customfreed of solvent on the rotary evaporator
  6. customis used without purification for the next reaction

출처 및 근거

ORD 기록
ord-77848d7e3975464fbb13ec4b9bd6c386
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084481B2

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