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Iodine → 9,10-dihydro-10-methyl-4-(1-methyl-4-piperidyl)-4H-benzo[4,5]cyclohepta-[1,2-b]thiophen-4-ol

HRID 27696
Notes
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Reaction equation

HRID 27696 reaction equation
II.Cl[CH:4]1[CH2:9][CH2:8][N:7]([CH3:10])[CH2:6][CH2:5]1.[CH3:11][CH:12]1[C:18]2[S:19][CH:20]=[CH:21][C:17]=2[C:16](=[O:22])[C:15]2[CH:23]=[CH:24][CH:25]=[CH:26][C:14]=2[CH2:13]1.[Cl-].[NH4+]>C(Br)CBr.O1CCCC1>[CH3:11][CH:12]1[C:18]2[S:19][CH:20]=[CH:21][C:17]=2[C:16]([CH:4]2[CH2:9][CH2:8][N:7]([CH3:10])[CH2:6][CH2:5]2)([OH:22])[C:15]2[CH:23]=[CH:24][CH:25]=[CH:26][C:14]=2[CH2:13]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 4

HCID 807IodineHCID 25517Ammonium ChlorideHCID 793424-chloro-N-methylpiperidineHCID 233418359,10-dihydro-10-methyl-4H-benzo[4,5]cyclohepta-[1,2-b]thiophen-4-one

Product 1

HCID 233418319,10-dihydro-10-methyl-4-(1-methyl-4-piperidyl)-4H-benzo[4,5]cyclohepta-[1,2-b]thiophen-4-ol

Reagents, catalysts & solvents 2

HCID 7839
1,2-Dibromoethane
Catalyst
HCID 8028TetrahydrofuranSolvent3×

Procedure

4.8 g of iodine-activated magnesium are covered with a layer of 60 cc of anhydrous tetrahydrofuran and cauterized with a few drops of ethylene bromide. A solution of 25.0 g of 4-chloro-1-methylpiperidine in 160 cc of anhydrous tetrahydrofuran is then added dropwise at such a rate that the solvent boils continually, and stirring is subsequently effected at the boil for 2 hours. The reaction mixture is cooled to 10°, and a solution of 20.0 g of 9,10-dihydro-10-methyl-4H-benzo[4,5]cyclohepta-[1,2-b]thiophen-4-one in 100 cc of anhydrous tetrahydrofuran is added dropwise at this temperature. After stirring at room temperature for 11/2 hours and at the boil for 30 minutes, the reaction mixture is cooled, poured on 300 cc of a 20% ammonium chloride solution, and the organic phase is separated. The aqueous solution is extracted with methylene chloride, the combined organic solutions are washed with water, dried over sodium sulphate and concentrated by evaporation. The 9,10-dihydro-10-methyl-4-(1-methyl-4-piperidyl)-4H-benzo[4,5]cyclohepta-[1,2-b]thiophen-4-ol, obtained as residue, is recrystallized twice from isopropanol. M.P. 177°-178°.

Workup

  1. temperatureThe reaction mixture is cooled to 10°
  2. stirringAfter stirring at room temperature for 11/2 hours
  3. waitat the boil for 30 minutes
  4. temperaturethe reaction mixture is cooled
  5. customthe organic phase is separated
  6. extractionThe aqueous solution is extracted with methylene chloride
  7. washthe combined organic solutions are washed with water
  8. dry with materialdried over sodium sulphate
  9. concentrationconcentrated by evaporation

Sources & evidence

ORD record
ord-9c631467525d4903ac5f362e53ff25fa
Source dataset
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04223035

Reaction notes

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