Hydrochloric Acid → HCID 12733982, compound
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]1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
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
- temperaturewas heated
- additionwere added
- temperaturethe mixture was again heated
- filtrationfiltered
- additionTo the cooled filtrate was added a N sodium hydroxide solution
- customthe precipitate formed
- filtrationwas filtered off
- customthen recrystallised from ethanol
Sources & evidence
- ORD record
- ord-fabec6d837e64ab5a8f8113481a8db97
- Source dataset
- uspto-grants-1984_04
- Patent number
- US04444776
Reaction notes
Loading…