1-Methylpiperazine → HCID 54044111, compound

HRID 372553Notes

Reaction equation

HRID 372553 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[O:8]=[C:9]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[CH2:13][CH2:12][CH:11]=[CH:10]1>C(O)C>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH:11]2[CH2:12][CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[C:9](=[O:8])[CH2:10]2)[CH2:4][CH2:3]1

Participants

4

Reactant 2

HCID 531671-MethylpiperazineHCID 9989489HCID 9989489, compound

Product 1

HCID 54044111HCID 54044111, compoundYield 85.3%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Conditions

Temperature
20 °C

Procedure

A solution of 8 g of N-methylpiperazine in 80 ml of ethanol was added over 5 minutes to a solution of 6.32 g of 5-oxo-8,9-dihydro [5H] benzocycloheptene in 40 ml of ethanol and the mixture was stirred for 4 hours at 20° C and was then evaporated to dryness. The residue was taken up in 0.5 N hydrochloric acid and the solution was washed with ethyl acetate and made alkaline with concentrated ammonium hydroxide. The mixture was extracted with methylene chloride and the extracts were dried and evaporated to dryness to obtain 8.8 g of 7-(4-methylpiperazin-1-yl)-5-oxo-6,7,8,9-tetrahydro [5H] benzocycloheptene.

Workup

  1. customwas then evaporated to dryness
  2. washthe solution was washed with ethyl acetate
  3. extractionThe mixture was extracted with methylene chloride
  4. customthe extracts were dried
  5. customevaporated to dryness

Sources & evidence

ORD record
ord-5664eeea6cf440ec95e5a32e7666e4f6
Source dataset
uspto-grants-1978_05
Patent number
US04091115

Reaction notes

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