反应详情

3-Chloromethyl-5,6-dimethoxy-1(1-trityl-4-imidazolyl)methyl-1H-indazole (165.0 g) was suspended in dimethyl sulfoxide (1200 ml) and the solution was stirred at room temperature. Then potassium cyanide (43.6 g), which had been ground in a mortar, was added thereto. After stirring at 70° C. for 1 hour, the reaction mixture became homogeneous and transparent. The reaction mixture was returned to room temperature and poured into water (15000 ml) while vigorously stirring. The stirring was continued for 1 hour. The solid thus precipitated was collected by filtration, washed with water (1000 ml×3), dissolved in chloroform (5000 ml), dried over sodium sulfate, filtered and evaporated under reduced pressure. The residue thus obtained was purified by using a silica gel column (ethyl acetate) to give 108.7 g of a pale brown solid. This solid product was used in the subsequent reaction without purification.

1. additionwas added
2. stirringAfter stirring at 70° C. for 1 hour
3. customwas returned to room temperature
4. stirringwhile vigorously stirring
5. customThe solid thus precipitated
6. filtrationwas collected by filtration
7. washwashed with water (1000 ml×3)
8. dissolutiondissolved in chloroform (5000 ml)
9. dry with materialdried over sodium sulfate
10. filtrationfiltered
11. customevaporated under reduced pressure
12. customThe residue thus obtained
13. customwas purified