HCID 23339765, compound → HCID 23339761, compound

HRID 28229Notes

Reaction equation

HRID 28229 reaction equation
C([N:11]1[CH2:25][CH2:24][N:14]2[C:15]3[N:23]=[CH:22][CH:21]=[CH:20][C:16]=3[NH:17][C:18](=[O:19])[CH:13]2[CH2:12]1)(OCC1C=CC=CC=1)=O>[Pd].C(O)C>[N:23]1[C:15]2[N:14]3[CH2:24][CH2:25][NH:11][CH2:12][CH:13]3[C:18](=[O:19])[NH:17][C:16]=2[CH:20]=[CH:21][CH:22]=1

Participants

4

Reactant 1

HCID 23339765HCID 23339765, compound

Product 1

HCID 23339761HCID 23339761, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 702EthanolSolvent

Procedure

A mixture of 1.5 g. of 8-carbobenzoxy-7,8,9,10-tetrahydro-5H-pyrazino[1,2-a]pyrido[3,2-e]pyrazin-6(6aH)-one, 1 g. of 10% palladium on carbon, and 150 ml. of ethanol is hydrogenated at 45 psi for 2 hours. The catalyst is filtered and the filtrate is concentrated. The residue is dissolved in a small amount of ethanol and ethanolic hydrogen chloride is added. Filtration of the precipitated salt gives 0.72 g. of the title product, m.p. 270° dec. Recrystallization from ethanol-water gives 0.60 g., m.p. 278°-279°.

Workup

  1. additionA mixture of 1.5 g
  2. filtrationThe catalyst is filtered
  3. concentrationthe filtrate is concentrated
  4. dissolutionThe residue is dissolved in a small amount of ethanol and ethanolic hydrogen chloride
  5. additionis added
  6. filtrationFiltration of the precipitated salt
  7. customgives 0.72 g

Sources & evidence

ORD record
ord-610a07d0806f4c4cb1731fa8a88b5787
Source dataset
uspto-grants-1980_09
Patent number
US04225713

Reaction notes

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