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Water → 4-n-butylthio-benzonitrile

HRID 394849
ノート
印刷プレビュー

反応式

HRID 394849 の反応式
Cl[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:16]([SH:20])[CH2:17][CH2:18][CH3:19].O>CC(N(C)C)=O>[CH2:16]([S:20][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1)[CH2:17][CH2:18][CH3:19]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8012ButanethiolHCID 11430Potassium CarbonateHCID 121634-Chlorobenzonitrile

生成物 1

HCID 110196724-n-butylthio-benzonitrile

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒2 回

反応条件

温度
80 °C

実験手順

To a well-stirred suspension of 41.27 g (0.3 mol) of 4-chlorobenzonitrile, 58.05 g (0.42 mol) of potassium carbonate and 200 ml DMA a solution of 27.06 g (0.3 mol) of 1-butanethiol in 50 ml of DMA are added under an atmosphere of nitrogen. The resulting mixture is heated to 80° C. and stirred at this temperature for 24 hours. Then, the reaction mixture is cooled to room temperature and poured into 750 ml of water. The crude product is extracted with 300 ml of ethyl acetate, washed with water, dried over MgSO4. Thereafter, ethyl acetate is removed. Then, fractional distillation yields 52.88 9 (80.4%) of colorless liquid 4-n-butylthio-benzonitrile.

後処理

  1. additionare added under an atmosphere of nitrogen
  2. temperatureThen, the reaction mixture is cooled to room temperature
  3. extractionThe crude product is extracted with 300 ml of ethyl acetate
  4. washwashed with water
  5. dry with materialdried over MgSO4
  6. customThereafter, ethyl acetate is removed
  7. distillationThen, fractional distillation

出典と根拠

ORDレコード
ord-d9f3e3f65d3948caaf50f5962f521157
出典データセット
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06603020B1

反応ノート

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