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Hydrochloric Acid → HCID 15686152、化合物

HRID 989467
ノート
印刷プレビュー

反応式

HRID 989467 の反応式
[OH-].[Na+].S(O[CH2:8][C:9]([NH2:12])([CH3:11])[CH3:10])(O)(=O)=O.[C:13]1([SH:19])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.Cl>O>[CH3:10][C:9]([NH2:12])([CH3:11])[CH2:8][S:19][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=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 313Hydrochloric AcidHCID 7969ThiophenolHCID 14798Sodium HydroxideHCID 2928692-Amino-2-methyl-1-propanol hydrogen sulfate

生成物 1

HCID 15686152HCID 15686152、化合物収率 57.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

In 5 ml of water was dissolved 0.20 g (5 mmol) of sodium hydroxide, followed by adding thereto 0.85 g (5 mmol) of 2-amino-2-methylpropyl hydrogensulfate and 0.66 g (6 mmol) of thiophenol, and the resulting mixture was stirred at 80° C. for 8 hours. After completion of the reaction, the reaction mixture was cooled to room temperature and acidified with 6N hydrochloric acid. The aqueous layer was washed with ethyl acetate and made basic with an aqueous sodium hydroxide solution, and the desired compound was extracted three times with ethyl acetate. The combined organic layer was washed with saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and then distilled under reduced pressure to remove the solvent, whereby 0.52 g of 2-methyl-1-phenylthio-2-propylamine was obtained (yield: 57%).

後処理

  1. additionby adding
  2. customAfter completion of the reaction
  3. washThe aqueous layer was washed with ethyl acetate
  4. extractionthe desired compound was extracted three times with ethyl acetate
  5. washThe combined organic layer was washed with saturated aqueous sodium chloride solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationdistilled under reduced pressure
  8. customto remove the solvent

出典と根拠

ORDレコード
ord-fb26ab19bd764e838633323bce452ece
出典データセット
uspto-grants-2003_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06639109B1

反応ノート

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