Reaktion #527667

Reaktionsgleichung

1-[1-(2-chlorophenyl)cyclopropyl]-6-fluoro-7-methoxy-2-methyl-1,2,3,4-tetrahydroisoquinoline

hydrobromic acid

→

1-[1-(2-chlorophenyl)cyclopropyl]-6-fluoro-7-hydroxy-2-methyl-1,2,3,4-tetrahydroisoquinoline hydrobromide

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturunder reflux under argon for 220 minutes
3. 3
   SonstigeThe solvent was removed in vacuo
4. 4
   Trocknenthe residue dried by azeotropic distillation with propan-2-ol
5. 5
   Sonstigecrystallised from propan-2-ol

Vorschrift

A mixture of 1-[1-(2-chlorophenyl)cyclopropyl]-6-fluoro-7-methoxy-2-methyl-1,2,3,4-tetrahydroisoquinoline (18.0 g) in acetic acid (150 ml) and 48% aqueous hydrobromic acid (150 ml) was heated under reflux under argon for 220 minutes. The solvent was removed in vacuo, and the residue dried by azeotropic distillation with propan-2-ol and crystallised from propan-2-ol to yield 1-[1-(2-chlorophenyl)cyclopropyl]-6-fluoro-7-hydroxy-2-methyl-1,2,3,4-tetrahydroisoquinoline hydrobromide (18.56 g), m.p. 240° C. (dec).

Quelle