1-Phenylpiperazine → HCID 21533325, compound

HRID 1657402Notes

Reaction equation

HRID 1657402 reaction equation
[C:1]1([N:7]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:14]([N:16]1[CH2:22][CH2:21][C:20]2[CH:23]=[CH:24][CH:25]=[CH:26][C:19]=2[CH2:18][O:17]1)=[O:15]>C(Cl)Cl>[C:1]1([N:7]2[CH2:12][CH2:11][N:10]([C:14]([N:16]3[CH2:22][CH2:21][C:20]4[CH:23]=[CH:24][CH:25]=[CH:26][C:19]=4[CH2:18][O:17]3)=[O:15])[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 70961-PhenylpiperazineHCID 21533324HCID 21533324, compound

Product 1

HCID 21533325HCID 21533325, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a solution of 4.22 g. (26 mmoles) of N-phenylpiperazine in CH2Cl2, 4.24 g. (20 mmoles) of 3-chlorocarbonyl-1,3,4,5-tetrahydro-2,3-benzoxazepine was added and the mixture was refluxed for 2 hours, cooled, washed with NaHCO3 and with H2O, dried over Na2SO4 and the solvent evaporated. Yield 5.5 g. (81.5%), m.p. 123°- 125°C, recrystallized from EtOH.

Workup

  1. temperaturethe mixture was refluxed for 2 hours
  2. temperaturecooled
  3. washwashed with NaHCO3 and with H2O
  4. dry with materialdried over Na2SO4
  5. customthe solvent evaporated
  6. custom(81.5%), m.p. 123°- 125°C, recrystallized from EtOH

Sources & evidence

ORD record
ord-5d9d02b528e14d878efd232349765abd
Source dataset
uspto-grants-1976_06
Patent number
US03960858

Reaction notes

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