Acetic Acid → Olopatadine Impurity 17
Reaction equation
C(C1[CH:18]=[CH:17][C:6]2[O:7][CH2:8][C:9]3[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=3[C:11](=[O:12])[C:5]=2[CH:4]=1)#N.Cl.[C:20]([OH:23])(=[O:22])[CH3:21]>O>[O:12]=[C:11]1[C:10]2[CH:13]=[CH:14][CH:15]=[CH:16][C:9]=2[CH2:8][O:7][C:6]2[CH:17]=[CH:18][C:21]([C:20]([OH:23])=[O:22])=[CH:4][C:5]1=2Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
Reflux 27.3 gm. of 2-cyano-6,11-dihydro-11-oxodibenz[b,e]oxepin in a mixture of 300 cc. of 37% aqueous hydrochloric acid and 300 cc. of glacial acetic acid for 24 hours. Cool, dilute with water and separate the solids by filtration in order to obtain the title product (m.p. 250° C. dec.).
Workup
- temperatureReflux 27.3 gm
- temperatureCool
- customseparate the solids
- filtrationby filtration in order
Sources & evidence
- ORD record
- ord-22b50447770248b19f472dbeb7d6785f
- Source dataset
- uspto-grants-1981_08
- Patent number
- US04282365
Reaction notes
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