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Acetone → HCID 13563677, 화합물

HRID 979721
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HRID 979721 반응식
CC(C)=O.[CH3:5][NH:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C(=O)([O-])[O-].[K+].[K+].Cl[C:20]([O:22][C:23]1[CH:28]=[CH:27][C:26]([Cl:29])=[C:25]([C:30]([CH3:33])([CH3:32])[CH3:31])[CH:24]=1)=[S:21]>O>[CH3:5][N:6]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:20](=[S:21])[O:22][C:23]1[CH:28]=[CH:27][C:26]([Cl:29])=[C:25]([C:30]([CH3:32])([CH3:31])[CH3:33])[CH:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 180Acetone2회HCID 7515N-MethylanilineHCID 11430Potassium CarbonateHCID 13563671HCID 13563671, 화합물

생성물 1

HCID 13563677HCID 13563677, 화합물수율 79.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 20 ml of acetone were added 1.07 g of N-methylaniline and 1.38 g of anhydrous potassium carbonate, and a solution obtained by dissolving 2.63 g of O-3-tert-butyl-4-chlorophenyl chlorothioformate into 20 ml of acetone was added thereto with stirring at room temperature. After stirring for 30 minutes as it is, the mixture was subjected to refluxing with heating for 2 hours. The reaction mixture was cooled down to room temperature and then poured into cold water. The product was extracted with benzene. The benzene solution was washed with water and a saturated aqueous solution of sodium chloride in this order, and dried over anhydrous magnesium sulfate. Thereafter, benzene was distilled off. The residue was purified through a column chromatography (employing silica gel as carrier, and benzene/hexane=1/1 (V/V) as developing solvent) and further recrystallized form ethanol to give 2.64 g of O-3-tert-butyl-4-chlorophenyl N-methyl-N-phenylthiocarbamate, having melting point of 65°-67° C.

후처리

  1. customa solution obtained
  2. additionwas added
  3. stirringAfter stirring for 30 minutes as it
  4. temperatureto refluxing
  5. temperaturewith heating for 2 hours
  6. temperatureThe reaction mixture was cooled down to room temperature
  7. extractionThe product was extracted with benzene
  8. washThe benzene solution was washed with water
  9. dry with materiala saturated aqueous solution of sodium chloride in this order, and dried over anhydrous magnesium sulfate
  10. distillationThereafter, benzene was distilled off
  11. customThe residue was purified through a column chromatography (employing silica gel as carrier, and benzene/hexane=1/1 (V/V) as developing solvent) and further recrystallized form ethanol

출처 및 근거

ORD 기록
ord-f2226b21e55e4c4c80e5532b826bd21a
출처 데이터셋
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04668831

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