Piperazine → HCID 21456041, compound

HRID 435688Notes

Reaction equation

HRID 435688 reaction equation
Cl[CH:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[S:6][C:5]2[CH:13]=[CH:14][C:15]([I:17])=[CH:16][C:4]=2[CH2:3]1.[NH:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1>[OH-].[Na+]>[I:17][C:15]1[CH:14]=[CH:13][C:5]2[S:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[CH:2]([N:18]3[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]3)[CH2:3][C:4]=2[CH:16]=1

Participants

4

Reactant 2

HCID 4837PiperazineHCID 12232368HCID 12232368, compound

Product 1

HCID 21456041HCID 21456041, compound

Reagents, catalysts & solvents 1

HCID 14798Sodium HydroxideSolvent

Procedure

10.1 g of 10-chloro-10,11-dihydro-2-iodo-dibenzo[b,f]thiepin and 23.3 g of piperazine are held at 120°-130° C for 1 hour. The mixture is cooled, diluted with 2-N sodium hydroxide and extracted with ether. The organic phase is washed with water until neutral and extracted with 500 ml of 2-N hydrochloric acid. The aqueous phase is made alkaline and extracted with chloroform. The organic phase is dried over magnesium sulphate and concentrated under reduced pressure. There is obtained 1-(10,11-dihydro-2-iodo-dibenzo[b,f]thiepin-10-yl)-piperazine as a brown oil.

Workup

  1. temperatureThe mixture is cooled
  2. extractionextracted with ether
  3. washThe organic phase is washed with water until neutral and
  4. extractionextracted with 500 ml of 2-N hydrochloric acid
  5. extractionextracted with chloroform
  6. dry with materialThe organic phase is dried over magnesium sulphate
  7. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-95534510156446a7acc0f11860e2282e
Source dataset
uspto-grants-1977_02
Patent number
US04006144

Reaction notes

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