Carbon Disulfide → 2,6-Xylyl isothiocyanate

HRID 65476

반응식

HRID 65476 반응식
[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]

참가 물질

8

반응물 4

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

생성물 1

HCID 879762,6-Xylyl isothiocyanate수율 74.7%

시약·촉매·용매 3

HCID 241Benzene용매HCID 962Water용매2회HCID 31374Dimethylacetamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-82b7b712d0e94545b1bc2ab0815b792f
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04614798

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