Hydrochloric Acid → HCID 20339418, compound

HRID 1395458Notes

Reaction equation

HRID 1395458 reaction equation
[N:1]1[CH:6]=[CH:5][C:4]([CH2:7][CH2:8][N:9]2[CH2:23][CH2:22][N:12]3[C:13]4[C:18]([NH:19][C:20](=[O:21])[CH:11]3[CH2:10]2)=[CH:17][CH:16]=[CH:15][CH:14]=4)=[CH:3][CH:2]=1.O.Cl.[H][H]>O=[Pt]=O.C(O)C>[NH:1]1[CH2:6][CH2:5][CH:4]([CH2:7][CH2:8][N:9]2[CH2:23][CH2:22][N:12]3[C:13]4[C:18]([NH:19][C:20](=[O:21])[CH:11]3[CH2:10]2)=[CH:17][CH:16]=[CH:15][CH:14]=4)[CH2:3][CH2:2]1

Participants

7

Reactant 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 20339411HCID 20339411, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 20339418HCID 20339418, compound

Reagents, catalysts & solvents 2

HCID 345198Adams' catalystCatalystHCID 702EthanolSolvent

Procedure

A solution of 2,3,4,4a-tetrahydro-3-[2-(4-pyridinyl)ethyl]-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one in 120 ml. water and 60 ml. ethanol containing 13 ml. conc. hydrochloric acid was placed in a Parr hydrogenation apparatus, with 1.2 g. PtO2, under 45 psi. of hydrogen and shaken till pressure drop ceased. After filtering off catalyst the solvents were removed under vacuum and the residue crystallized from hot ethanol. Product filtered off, washed (ethanol), and dried. Dissolved in hot methanol which was displaced by ethanol by boiling off lower boiling solvent. Yield: 4.0 g. of the title compound as the dihydrochloride salt, m.p. 238°-240° C.

Workup

  1. filtrationAfter filtering off catalyst the solvents
  2. customwere removed under vacuum
  3. customthe residue crystallized from hot ethanol
  4. filtrationProduct filtered off
  5. washwashed (ethanol)
  6. customdried
  7. dissolutionDissolved in hot methanol which

Sources & evidence

ORD record
ord-b528c5ff6d5943b2a2668f6e2c0371e7
Source dataset
uspto-grants-1980_05
Patent number
US04203987

Reaction notes

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