反应详情

The product of stage (b) was suspended in 10 ml of boiling methanol and 0.55 g of potassium hydroxide in 5.5 ml of water was added dropwise over 15 mins. The mixture was refluxed until a dark red solution formed, (after ca. 6 hrs) when 2 ml of concentrated hydrochloric acid was cautiously added dropwise. The mixture was cooled and filtered, and the solid residue washed thoroughly with water. The water washings were re-acidified and filtered. The combined solid residues (500 mg) mp 200°-209°, were recrystallised from acetonitrile to give the title product as the trans-isomer (300 mg) m.p. 216°-219° C.

1. temperatureThe mixture was refluxed until a dark red solution
2. customformed
3. temperatureThe mixture was cooled
4. filtrationfiltered
5. washthe solid residue washed thoroughly with water
6. filtrationfiltered
7. customThe combined solid residues (500 mg) mp 200°-209°, were recrystallised from acetonitrile