Hydrochloric Acid → 90060-20-1

HRID 1636641Notes

Reaction equation

HRID 1636641 reaction equation
Br.[OH:2][C:3]1[C:12]([OH:13])=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][CH:7]([NH:15][CH3:16])[C:8]2=O.[ClH:17]>[Pd].O>[ClH:17].[OH:2][C:3]1[C:12]([OH:13])=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][CH:7]([NH:15][CH3:16])[CH2:8]2

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 12353635HCID 12353635, compound

Product 1

HCID 691848290060-20-1

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 962WaterSolvent

Conditions

Temperature
0 °C

Procedure

A mixture of 10.0 g of 5,6-dihydroxy-2-methylamino-1-tetralone hydrobromide, 2.0 g of Pd/C 5%, 90 ml of water and 10 ml of 37% HCl is hydrogenated in an autoclave (Hastelloy) (20 atm, 80° C.) for 8-9 hours, then is filtered washing with hot water. The aqueous solution is concentrated under vacuum and the resulting solid is warm triturated with 100 ml of 37% hydrochloric acid, then cooled to 0° C. and filtered. The resulting solid is recrystallized from acetone and dried under vacuum at 60° C. Yield: 7.4 g.

Workup

  1. filtrationis filtered
  2. washwashing with hot water
  3. concentrationThe aqueous solution is concentrated under vacuum
  4. temperaturethe resulting solid is warm
  5. customtriturated with 100 ml of 37% hydrochloric acid
  6. filtrationfiltered
  7. customThe resulting solid is recrystallized from acetone
  8. customdried under vacuum at 60° C

Sources & evidence

ORD record
ord-3c7f8153ace74d128cd633f2b040357f
Source dataset
uspto-grants-2000_03
Patent number
US06034277

Reaction notes

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