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Water → HCID 12097381、化合物

HRID 989468
ノート
印刷プレビュー

反応式

HRID 989468 の反応式
O.C(=O)([O-])[O-].[K+].[K+].S(O[CH2:13][C:14]([NH2:17])([CH3:16])[CH3:15])(O)(=O)=O.[CH2:18]([SH:26])[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]>C(O)C>[CH3:15][C:14]([NH2:17])([CH3:16])[CH2:13][S:26][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]
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 962WaterHCID 81441-OctanethiolHCID 11430Potassium CarbonateHCID 2928692-Amino-2-methyl-1-propanol hydrogen sulfate

生成物 1

HCID 12097381HCID 12097381、化合物収率 100%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In a mixed solvent of 10 ml of water and 10 ml of ethanol was suspended 1.38 g (10 mmol) of potassium carbonate. To the suspension were added 0.85 g (5 mmol) of 2-amino-2-methylpropyl hydrogensulfate and 0.73 g (5 mmol) of 1-octanethiol, and the resulting mixture was gently refluxed for 8 hours. After completion of the reaction, the reaction mixture was cooled to room temperature 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 1.08 g of 2-methyl-1-n-octylthio-2-propylamine was obtained. The purity was measured in terms of area percentage by gas chromatography and found to be 91%.

後処理

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

出典と根拠

ORDレコード
ord-4b50b85bcdb649c2860d9ebdf3a816df
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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