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Acetone → HCID 13563677、化合物

HRID 979721
ノート
印刷プレビュー

反応式

HRID 979721 の反応式
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
参加物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 180Acetone2 回HCID 7515N-MethylanilineHCID 11430Potassium CarbonateHCID 13563671HCID 13563671、化合物

生成物 1

HCID 13563677HCID 13563677、化合物収率 79.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f2226b21e55e4c4c80e5532b826bd21a
出典データセット
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04668831

反応ノート

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