Hydrochloric Acid → HCID 12733982, compound

HRID 326115Notes

Reaction equation

HRID 326115 reaction equation
[O:1]=[C:2]1[C:11]2[C:6](=[C:7]([CH3:17])[C:8]([NH:13]C(=O)C)=[CH:9][C:10]=2[CH3:12])[CH:5]=[CH:4][NH:3]1.C(O)C.Cl>O>[O:1]=[C:2]1[C:11]2[C:6](=[C:7]([CH3:17])[C:8]([NH2:13])=[CH:9][C:10]=2[CH3:12])[CH:5]=[CH:4][NH:3]1

Participants

5

Procedure

The mixture consisting of 10.6 g of the compound G, 175 ml of ethanol and 35 ml of concentrated hydrochloric acid was heated with reflux for 21/2 hours, 300 ml of water were added, the mixture was again heated to boiling point and filtered to eliminate a small insoluble fraction. To the cooled filtrate was added a N sodium hydroxide solution to bring the pH to 9 and the precipitate formed was filtered off then recrystallised from ethanol to give 7.35 g (85%) of cream flakes corresponding to the amine of formula H, melting point 242° C.

Workup

  1. temperaturewas heated
  2. additionwere added
  3. temperaturethe mixture was again heated
  4. filtrationfiltered
  5. additionTo the cooled filtrate was added a N sodium hydroxide solution
  6. customthe precipitate formed
  7. filtrationwas filtered off
  8. customthen recrystallised from ethanol

Sources & evidence

ORD record
ord-fabec6d837e64ab5a8f8113481a8db97
Source dataset
uspto-grants-1984_04
Patent number
US04444776

Reaction notes

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