Hydrochloric Acid → 65008-41-5

HRID 1155574Notes

Reaction equation

HRID 1155574 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:33]=[CH:34][C:35]=1[O:36][CH3:37])[CH2:6][CH2:7][NH:8][CH2:9][CH:10]([OH:32])[CH2:11][O:12][C:13]1[CH:22]=[CH:21][C:20]([O:23]CC2C=CC=CC=2)=[C:19]2[C:14]=1[CH2:15][CH2:16][C:17](=[O:31])[NH:18]2.C(O)C.[ClH:41]>CO.[C].[Pd]>[ClH:41].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:33]=[CH:34][C:35]=1[O:36][CH3:37])[CH2:6][CH2:7][NH:8][CH2:9][CH:10]([OH:32])[CH2:11][O:12][C:13]1[CH:22]=[CH:21][C:20]([OH:23])=[C:19]2[C:14]=1[CH2:15][CH2:16][C:17](=[O:31])[NH:18]2

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 12751756HCID 12751756, compound

Product 1

HCID 304954365008-41-5

Reagents, catalysts & solvents 2

HCID 178418390HCID 178418390, compoundCatalystHCID 887MethanolSolvent

Procedure

2.0 g of 5-[3-(3,4-dimethoxyphenethylamino)-2-hydroxypropoxy]-8-benzyloxy-3,4-dihydrocarbostyril was suspended in 50 ml of methanol, and ethanol containing hydrogen chloride was added to the suspension until the suspension showed acidity to form a homogeneous solution. 0.7 g of 10% palladium carbon was added to the resulting solution, and the mixture was stirred at room temperature and at atmospheric pressure to absorb hydrogen. The reaction completed at the point when the absorption of hydrogen ceased. The catalyst was removed by filtration, and the methanol evaporated. To the residue was added a small amount of ethanol to crystallized followed by recrystallization from ethanol to obtain 1.5 g of 5-[3-(3,4-dimethoxyphenethylamino)-2-hydroxypropoxy]-8-hydroxy-3,4-dihydrocarbostyril hydrochloride as colorless powdery crystals having a melting point of 171°-173° C.

Workup

  1. additionwas added to the suspension until the suspension
  2. customto form a homogeneous solution
  3. customto absorb hydrogen
  4. customthe absorption of hydrogen
  5. customThe catalyst was removed by filtration
  6. customthe methanol evaporated
  7. additionTo the residue was added a small amount of ethanol
  8. customto crystallized
  9. customfollowed by recrystallization from ethanol

Sources & evidence

ORD record
ord-7c225f36246c4c1aabca1c4c59035bd9
Source dataset
uspto-grants-1981_11
Patent number
US04302588

Reaction notes

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