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

HRID 660888ノート

反応式

HRID 660888 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒2 回HCID 6344Dichloromethane溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-77848d7e3975464fbb13ec4b9bd6c386
出典データセット
uspto-grants-2011_12
特許番号
US08084481B2

反応ノート

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