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Potassium Hydroxide → 5-Methyl-2,3-dihydro-1,4-benzothiazepine

HRID 539954
ノート
印刷プレビュー

反応式

HRID 539954 の反応式
[SH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=O)[CH3:9].[OH-].[K+].Br.Br[CH2:15][CH2:16][NH2:17]>C(O)C>[CH3:9][C:8]1[C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[S:1][CH2:15][CH2:16][N:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 27742172-Bromoethylamine hydrobromideHCID 110948191-(2-Sulfanylphenyl)ethan-1-one

生成物 1

HCID 200722975-Methyl-2,3-dihydro-1,4-benzothiazepine収率 79.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 1-(2-sulfanylphenyl)ethanone (6.40 g, 42.05 mmol) in ethanol (80 mL) was added an aqueous solution of potassium hydroxide (7.08 g, 126.14 mmol in 30 mL of water) and an aqueous solution of 2-bromoethanamine hydrobromide (9.48 g, 46.25 mmol in 30 mL of water). After being stirred at room temperature for 6 hours, the reaction mixture was concentrated in vacuo to remove most of ethanol and extracted with dichloromethane (60 mL×3). The combined organic layers were washed with brine (100 mL), dried over anhydrous sodium sulfate, and concentrated in vacuo. The residue was purified by flash column chromatography to give 5.92 g of 5-methyl-2,3-dihydro-1,4-benzothiazepine.

後処理

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. customto remove most of ethanol
  3. extractionextracted with dichloromethane (60 mL×3)
  4. washThe combined organic layers were washed with brine (100 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by flash column chromatography

出典と根拠

ORDレコード
ord-0184d1ea78ce40eaa972cb24ba19dc1e
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08871756B2

反応ノート

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