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

HRID 539954
Notes
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Reaction equation

HRID 539954 reaction equation
[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
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

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

Product 1

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

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

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.

Workup

  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

Sources & evidence

ORD record
ord-0184d1ea78ce40eaa972cb24ba19dc1e
Source dataset
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08871756B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes