1-Methylpiperazine → HCID 22767842, compound

HRID 437835Notes

Reaction equation

HRID 437835 reaction equation
Cl[CH:2]1[C:8]2[CH:9]=[C:10]([CH3:13])[CH:11]=[CH:12][C:7]=2[O:6][C:5]2[CH:14]=[CH:15][C:16]([CH3:18])=[CH:17][C:4]=2[CH2:3]1.[CH3:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>C(Cl)(Cl)Cl>[CH3:18][C:16]1[CH:15]=[CH:14][C:5]2[O:6][C:7]3[CH:12]=[CH:11][C:10]([CH3:13])=[CH:9][C:8]=3[CH:2]([N:23]3[CH2:24][CH2:25][N:20]([CH3:19])[CH2:21][CH2:22]3)[CH2:3][C:4]=2[CH:17]=1

Participants

4

Reactant 2

HCID 531671-MethylpiperazineHCID 2276790610-Chloro-10,11-dihydro-2,8-dimethyl-dibenz[b,f]oxepin

Product 1

HCID 22767842HCID 22767842, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

0.8 G. of 10-chloro-10,11-dihydro-2,8-dimethyl-dibenz[b,f]oxepin and 0.58 g. of 1-methyl-piperazine are dissolved in 4 ml. of chloroform and heated at reflux for 21 hours. Then, the chloroform is evaporated in vacuo. The residue is partitioned between benzene and aqueous sodium carbonate solution. The benzene solution is extracted with dilute hydrochloric acid. The hydrochloric acid extract is made alkaline with sodium carbonate and extracted with benzene. Thereafter, the benzene extract is washed several times with water, dried over sodium sulfate, evaporated in vacuo, and there is obtained 1-[10,11-dihydro-2,8-dimethyl-dibenz[ b,f]oxepin-10-yl] -4-methyl-piperazine, the dihydrochloride of which melts at 197°- 198° C. (with decomposition).

Workup

  1. temperatureat reflux for 21 hours
  2. customThen, the chloroform is evaporated in vacuo
  3. customThe residue is partitioned between benzene and aqueous sodium carbonate solution
  4. extractionThe benzene solution is extracted with dilute hydrochloric acid
  5. extractionThe hydrochloric acid extract
  6. extractionextracted with benzene
  7. extractionThereafter, the benzene extract
  8. washis washed several times with water
  9. dry with materialdried over sodium sulfate
  10. customevaporated in vacuo

Sources & evidence

ORD record
ord-b8e6739e87ae4907982fd7fe467eef6c
Source dataset
uspto-grants-1977_06
Patent number
US04032525

Reaction notes

Loading…