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Sulfuric Acid → HCID 86623120、化合物

HRID 548784
ノート
印刷プレビュー

反応式

HRID 548784 の反応式
[CH2:1]([O:3][CH:4]([CH3:7])[CH2:5][NH2:6])[CH3:2].C([N:16]=[C:17]=[S:18])(=O)C1C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+].S(=O)(=O)(O)O>C(Cl)(Cl)Cl>[CH2:1]([O:3][CH:4]([CH3:7])[CH2:5][NH:6][C:17]([NH2:16])=[S:18])[CH3:2]
参加物反応条件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 1118Sulfuric AcidHCID 11430Potassium CarbonateHCID 68284Benzoyl isothiocyanateHCID 224502832-Ethoxypropan-1-amine

生成物 1

HCID 86623120HCID 86623120、化合物収率 68%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
75 °C

実験手順

2-Ethoxy-propylamine (1.50 g, 14.5 mmol) and benzoylisothiocyanate (2.61 g, 16.0 mmol) in chloroform (50 mL) were heated at 75° C. for 1 h. The solvent was removed under reduced pressure and methanol (15 mL) and water (30 mL) were added. Potassium carbonate (2.0 g, 14.5 mmol) was added and the mixture was heated at 75° C. for 2 h. After cooling to room temperature, the mixture was neutralized with 2M sulphuric acid and the solvent was removed under reduced pressure. The crude product was dissolved in methanol and insoluble material was removed by filtration. The solvent was distilled off and the resulting solid was washed with dichloromethane and dissolved in ethanol. Insoluble material was removed by filtration and the solvent was removed under reduced pressure. This gave the title compound as a white solid (1.6 g, 59% yield).

後処理

  1. customThe solvent was removed under reduced pressure and methanol (15 mL) and water (30 mL)
  2. additionwere added
  3. temperatureAfter cooling to room temperature
  4. customthe solvent was removed under reduced pressure
  5. dissolutionThe crude product was dissolved in methanol
  6. custominsoluble material was removed by filtration
  7. distillationThe solvent was distilled off
  8. washthe resulting solid was washed with dichloromethane
  9. dissolutiondissolved in ethanol
  10. customInsoluble material was removed by filtration
  11. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-fe498ca40f2543dd80ffe58a0d6c2ed6
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07943625B2

反応ノート

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