Water → 4-(Methylthio)thiobenzamide

HRID 1178579ノート

反応式

HRID 1178579 の反応式
[CH3:1][S:2][C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[CH:5][CH:4]=1.P([S-])(OCC)(OCC)=[S:12].O>Cl.C(OCC)(=O)C>[CH3:1][S:2][C:3]1[CH:10]=[CH:9][C:6]([C:7]([NH2:8])=[S:12])=[CH:5][CH:4]=1

参加物

6

反応物 3

HCID 962WaterHCID 5909604-(Methylthio)benzonitrileHCID 1385274Diethyl dithiophosphate, potassium salt

生成物 1

HCID 30033144-(Methylthio)thiobenzamide収率 67%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 8857Ethyl Acetate溶媒

実験手順

4-Methylthiobenzonitrile (12 g) was dissolved in a 4N solution of hydrogen chloride in ethyl acetate (130 mL). To this solution was added O,O-diethyl dithiophosphate (15 mL) and the mixture was stirred at room temperature for 22 hours. Water (100 mL) was added to the reaction mixture and extracted with ethyl acetate. After the insoluble materials were filtered off, the filtrate was washed with a saturated aqueous solution of sodium chloride and dried and, thereafter, the solvent was distilled off. The residue was recrystallized from ethyl acetate to obtain 10 g of the title compound (yield 67%).

後処理

  1. extractionextracted with ethyl acetate
  2. filtrationAfter the insoluble materials were filtered off
  3. washthe filtrate was washed with a saturated aqueous solution of sodium chloride
  4. customdried
  5. distillationthe solvent was distilled off
  6. customThe residue was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-d441511b1260476ca4ebd7a89c7cc3a5
出典データセット
uspto-grants-2007_10
特許番号
US07276527B2

反応ノート

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