Hydrochloric Acid → HCID 19352270, compound

HRID 726884Notes

Reaction equation

HRID 726884 reaction equation
[ClH:1].[CH3:2][O:3][C:4]1[C:13]([O:14][CH3:15])=[CH:12][CH:11]=[C:10]2[C:5]=1[CH2:6][CH2:7][CH:8]([NH:17][CH3:18])[C:9]2=O.Cl>[Pd].C(O)C>[ClH:1].[CH3:2][O:3][C:4]1[C:13]([O:14][CH3:15])=[CH:12][CH:11]=[C:10]2[C:5]=1[CH2:6][CH2:7][CH:8]([NH:17][CH3:18])[CH2:9]2

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 19352275HCID 19352275, compound

Product 1

HCID 19352270HCID 19352270, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 702EthanolSolvent

Procedure

14.0 g of 5,6-dimethoxy-2-methylamino-1-tetralone hydrochloride (0.051 mole), 400 ml of absolute ethanol, 10 ml of 1M methanolic HCl and 4.0 g of 5% Pd/C are placed into an autoclave (50% humidity), then the mixture is hydrogenated (P about 7 atm., T=80° C.) with stirring for 24 hours. The mixture is filtered, washing thoroughly the filtration cake with hot methanol, then the alcoholic solution is evaporated to dryness. The resulting solid is taken up into 150 ml of acetone, then the precipitate is filtered and dried under vacuum at 60° C. Yield: 10.8 g, 82% (moles), 77% (weight); M.p.=219°-220° C.

Workup

  1. custom(P about 7 atm., T=80° C.)
  2. filtrationThe mixture is filtered
  3. washwashing thoroughly the filtration cake with hot methanol
  4. customthe alcoholic solution is evaporated to dryness
  5. filtrationthe precipitate is filtered
  6. customdried under vacuum at 60° C

Sources & evidence

ORD record
ord-af1e85d312534d859422c220852946b4
Source dataset
uspto-grants-1998_01
Patent number
US05710336

Reaction notes

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