Piperazine → HCID 13688004, compound

HRID 2290282Notes

Reaction equation

HRID 2290282 reaction equation
Cl[CH:2]1[C:12]2[C:6]([CH:7]=[CH:8][CH:9]=[C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]3=2)=[CH:5][CH:4]=[CH:3]1.[NH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1>C(Cl)(Cl)Cl>[CH:16]1[C:10]2[CH:9]=[CH:8][C:7]3[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=3[CH:12]([N:17]3[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]3)[C:11]=2[CH:13]=[CH:14][CH:15]=1

Participants

4

Reactant 2

HCID 4837PiperazineHCID 86741066HCID 86741066, compound

Product 1

HCID 13688004HCID 13688004, compoundYield 100%

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent2×

Procedure

The chlorodibenzocycloheptene intermediate thus prepared was dissolved in 50 milliliters of chloroform, the solution added dropwise to a solution of 41.3 grams (480 millimoles) of piperazine in 150 milliliters of chloroform and the resulting mixture stirred for two days. At the end of this time, the mixture was washed successively with 20 percent sodium hydroxide, water, and brine, then dried over potassium carbonate. The drying agent was filtered off and the solvent vaporized to obtain 6.70 grams (100 percent yield) of 4-(5H-dibenzo[a,d]cyclohepten-5-yl)piperazine product as residue. A portion of the product was recrystallized from acetonitrile to obtain a purified product, m.p. 139°-141° C. Elemental analyses of the product after drying for 24 hours at 65° C. at 20 millimeters of mercury pressure were as follows:

Workup

  1. washAt the end of this time, the mixture was washed successively with 20 percent sodium hydroxide, water, and brine
  2. dry with materialdried over potassium carbonate
  3. filtrationThe drying agent was filtered off

Sources & evidence

ORD record
ord-9f130dd2e459414ea979cab6432a84df
Source dataset
uspto-grants-1986_10
Patent number
US04616023

Reaction notes

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