反应详情

A 50 mg portion of 2-hydroxy-4-methoxyaniline hydrochloride dissolved in 15 ml of ethanol was mixed with 16 mg of potassium hydroxide. After 10 minutes of reaction, to this was added 50 ml of carbon disulfide to carry out 24 hours of heating under reflux. The reaction mixture was concentrated under a reduced pressure, and the resulting residue was dissolved in 100 ml of dichloromethane, washed with water, dehydrated with magnesium sulfate and then concentrated under a reduced pressure. The resulting residue was purified by a silica gel column chromatography (dichloromethane:methanol=30:1) to obtain 46 mg of 6-methoxy-2-mercaptobenzoxazole.

1. customAfter 10 minutes of reaction
2. temperatureof heating
3. temperatureunder reflux
4. concentrationThe reaction mixture was concentrated under a reduced pressure
5. dissolutionthe resulting residue was dissolved in 100 ml of dichloromethane
6. washwashed with water
7. concentrationconcentrated under a reduced pressure
8. customThe resulting residue was purified by a silica gel column chromatography (dichloromethane:methanol=30:1)