Hydrochloric Acid → HCID 23171025, compound
Reaction equation
[NH2:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[NH2:12])[NH:8][C:7](=[O:13])[CH2:6][C:5]2([CH3:15])[CH3:14].[C:16](OC(=O)C)(=O)[CH3:17].Cl>C(O)C>[CH3:16][C:17]1[NH:1][C:2]2=[CH:3][C:4]3[C:5]([CH3:15])([CH3:14])[CH2:6][C:7](=[O:13])[NH:8][C:9]=3[CH:10]=[C:11]2[N:12]=1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
3.1 g. 6,7-diamino-4,4-dimethyl-1,2,3,4-tetrahydro- quinolin-2-one and 2.8 ml. acetic anhydride were stirred in 50 ml. ethanol for 30 minutes at ambient temperature. 20 ml. concentrated hydrochloric acid were then added thereto and the reaction mixture refluxed for 18 hours. The solvent was removed in a vacuum and the residue was dissolved in water, rendered alkaline with ammonia, filtered off with suction and washed with water. After recrystallisation from ethyl acetate, there were obtained 2.4 g. of the title compound; m.p. 290 294° C.
Workup
- temperaturethe reaction mixture refluxed for 18 hours
- customThe solvent was removed in a vacuum
- dissolutionthe residue was dissolved in water
- filtrationfiltered off with suction
- washwashed with water
- customAfter recrystallisation from ethyl acetate
- customthere were obtained 2.4 g
Sources & evidence
- ORD record
- ord-120cf148a07f473b9652b4543499d027
- Source dataset
- uspto-grants-1990_09
- Patent number
- US04954498
Reaction notes
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