1-Methylpiperazine → HCID 3041883, compound

HRID 1658742Notes

Reaction equation

HRID 1658742 reaction equation
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]2[S:6][C:7]3[CH:15]=[C:14]([F:16])[CH:13]=[CH:12][C:8]=3[CH:9](Cl)[CH2:10][C:4]=2[CH:3]=1.[CH3:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>>[Cl:1][C:2]1[CH:18]=[CH:17][C:5]2[S:6][C:7]3[CH:15]=[C:14]([F:16])[CH:13]=[CH:12][C:8]=3[CH:9]([N:23]3[CH2:24][CH2:25][N:20]([CH3:19])[CH2:21][CH2:22]3)[CH2:10][C:4]=2[CH:3]=1

Participants

3

Reactant 2

HCID 531671-MethylpiperazineHCID 12232369HCID 12232369, compound

Product 1

HCID 3041883HCID 3041883, compound

Procedure

12 g of 2,10-dichloro-7-fluoro-10,11-dihydro-dibenzo[b,f]thiepin are heated for 10 minutes together with 16 g of N-methylpiperazine at an external temperature of 120°-130°. After cooling the reaction mixture is poured on water and extracted with ether. The organic phase is washed with water and subsequently treated with 2 N hydrochloric acid. A precipitate is obtained. The mixture is extracted with ether, made alkaline and subsequently again extracted with ether. The organic phase is washed with water, dried over magnesium sulphate and evaporated. The so-obtained raw 1-(2-chloro-7-fluoro-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-4-methylpiperazine is converted to the corresponding maleate by treatment with maleic acid. The maleat melts at 200° with decomposition.

Workup

  1. temperatureAfter cooling the reaction mixture
  2. additionis poured on water
  3. extractionextracted with ether
  4. washThe organic phase is washed with water
  5. additionsubsequently treated with 2 N hydrochloric acid
  6. customA precipitate is obtained
  7. extractionThe mixture is extracted with ether
  8. extractionsubsequently again extracted with ether
  9. washThe organic phase is washed with water
  10. dry with materialdried over magnesium sulphate
  11. customevaporated

Sources & evidence

ORD record
ord-6464a597edb64584a82d22adb9e1724a
Source dataset
uspto-grants-1976_06
Patent number
US03966737

Reaction notes

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