HCID 20378662, compound → HCID 20378672, compound

HRID 1390372Notes

Reaction equation

HRID 1390372 reaction equation
[NH2:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]1[CH2:12][CH2:13][N:14](C(OCC3C=CC=CC=3)=O)[CH2:15][CH:7]1[C:6](=[O:26])[NH:5]2>[Pd].C(O)C>[NH2:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]1[CH2:12][CH2:13][NH:14][CH2:15][CH:7]1[C:6](=[O:26])[NH:5]2

Participants

4

Reactant 1

HCID 20378662HCID 20378662, compound

Product 1

HCID 20378672HCID 20378672, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 702EthanolSolvent

Procedure

A mixture of 1.5 g. of 8-amino-3-carbobenzoxy-2,3,4,4a-tetrahydro-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one, 1.5 g. of 10% Palladium on carbon catalyst and 150 ml. of ethanol is hydrogenated for 1/2 hour at 45 p. s. i. The catalyst is filtered and the filtrate concentrated to a volume of 50 ml. Ethanolic hydrochloric acid is added, and the product precipitates as the hydrochloride salt. Weight of product 0.70 g., m.p. 294-295° dec. Recrystallization from ethanol-water gives 0.45 g. of pure product, m.p. 315-317° dec.

Workup

  1. additionA mixture of 1.5 g
  2. filtrationThe catalyst is filtered
  3. concentrationthe filtrate concentrated to a volume of 50 ml
  4. additionEthanolic hydrochloric acid is added
  5. customthe product precipitates as the hydrochloride salt
  6. customRecrystallization from ethanol-water
  7. customgives 0.45 g

Sources & evidence

ORD record
ord-d413e27853c04a0b8e841c4a238ad975
Source dataset
uspto-grants-1979_02
Patent number
US04138567

Reaction notes

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