Carbon Disulfide → 2,6-Xylyl isothiocyanate

HRID 65476

反応式

HRID 65476 の反応式
[H-].[Na+].[CH3:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH3:10])[C:5]=1[NH:11][C:12](=O)C.[H][H].C(=S)=[S:18]>O.C1C=CC=CC=1.CC(N(C)C)=O>[CH3:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH3:10])[C:5]=1[N:11]=[C:12]=[S:18]

参加物

8

反応物 4

HCID 6348Carbon DisulfideHCID 16616N-Acetyl-2,6-xylidineHCID 24758Sodium hydrideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 879762,6-Xylyl isothiocyanate収率 74.7%

試薬・触媒・溶媒 3

HCID 241Benzene溶媒HCID 962Water溶媒2 回HCID 31374Dimethylacetamide溶媒

実験手順

To a suspension of 2.5 g (0.05 mol) of sodium hydride in a mixture of 40 ml of dry-dimethylacetamide and 40 ml of dry benzene, 0.05 mole of N-(2,6-dimethylphenyl)acetamide was added. After evolution of hydrogen ceased, the mixture was cooled in ice and water, and with stirring 0.075 mole of carbon disulfide was added slowly. The mixture was stirred at room temperature for 20 minutes. The reaction mixture was poured into water and extracted with toluene. The organic layer, dried over sodium sulfate, was evaporated, and distillation of the residue yielded 6.1 g (74%) of 2,6-dimethylphenylisothiocyanate.

後処理

  1. additionin a mixture of 40 ml
  2. additionwas added
  3. temperaturethe mixture was cooled in ice
  4. additionwas added slowly
  5. extractionextracted with toluene
  6. dry with materialThe organic layer, dried over sodium sulfate
  7. customwas evaporated
  8. distillationdistillation of the residue

出典と根拠

ORDレコード
ord-82b7b712d0e94545b1bc2ab0815b792f
出典データセット
uspto-grants-1986_09
特許番号
US04614798

関連ノート

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