Acetic Acid → HCID 21558510, compound

HRID 1578702Notes

Reaction equation

HRID 1578702 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][C:5](=O)[CH2:4][CH2:3]1.C(O)(=O)C.[NH2:13][C:14]1[CH:19]=[C:18]([Cl:20])[C:17]([Cl:21])=[CH:16][C:15]=1[N:22]1[CH:26]=[CH:25][CH:24]=[CH:23]1>C(O)C>[Cl:20][C:18]1[CH:19]=[C:14]2[C:15](=[CH:16][C:17]=1[Cl:21])[N:22]1[CH:23]=[CH:24][CH:25]=[C:26]1[C:5]1([CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1)[NH:13]2

Participants

5

Reactant 3

HCID 176Acetic AcidHCID 740491-Methyl-4-piperidoneHCID 10775663HCID 10775663, compound

Product 1

HCID 21558510HCID 21558510, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

3.39 g (0.03 mole) of 1-methyl-4-piperidone and 5 ml. of glacial acetic acid are added to a solution of 6.81 g (0.03 mole) of 1-(2-amino-4,5-dichlorophenyl)pyrrole in 100 ml. of absolute ethanol. The solution is refluxed for 50 hours and concentrated, and the residue is dissolved in water. The solution is filtered and basified. A solid precipitates and is filtered, dried, and recrystallized from ethanol to give 7,8-dichloro-4,5-dihydro-1'-methylspiro[pyrrolo(1,2-a)quinoxaline-4,4'-piperidine], m.p. 214°-215° C.

Workup

  1. temperatureThe solution is refluxed for 50 hours
  2. concentrationconcentrated
  3. dissolutionthe residue is dissolved in water
  4. filtrationThe solution is filtered
  5. customA solid precipitates
  6. filtrationis filtered
  7. customdried
  8. customrecrystallized from ethanol

Sources & evidence

ORD record
ord-293d9460c78f45c1b45b98b0aae97b72
Source dataset
uspto-grants-1976_02
Patent number
US03939159

Reaction notes

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