Reaction #2146761

Reaction equation

7-Chloro-6-fluoro-isoquinoline

3-Chloro-benzene-carboperoxoic acid

→

material

Yield 67.6%

7-Chloro-6-fluoro-isoquinoline 2-oxide

Yield 67.6%

Solvents

dichloromethane

Conditions

Workup

1. 1
   FiltrationFor workup, the precipitate was filtered off
2. 2
   Washwashed with dichloromethane
3. 3
   WashThe filtrate was washed twice with NaHCO3-solution
4. 4
   OtherThe layers were separated
5. 5
   Extractionthe aqueous phase was extracted twice with dichloromethane
6. 6
   DryingThe organic phases were dried with MgSO4
7. 7
   Otherevaporated

Procedure

25 g (137.7 mmol) of 7-Chloro-6-fluoro-isoquinoline (3) were in dissolved in 500 ml of dichloromethane. At room temperature 50.9 g (206.5 mmol) of 3-Chloro-benzene-carboperoxoic acid (70%) were added and the mixture was stirred at room temperature until complete conversion is achieved. For workup, the precipitate was filtered off and washed with dichloromethane. The filtrate was washed twice with NaHCO3-solution. The layers were separated and the aqueous phase was extracted twice with dichloromethane. The organic phases were dried with MgSO4 and evaporated. The so obtained solid material (18.4 g) was used without further purification. Rt=0.87 min (Method C). Detected mass: 198.1/200.1 (M+H+).

Source