反应详情

To a mixture of LiH (12.6 g) and HMPA (105 mi) in DMF (1050 mi) at 0° C. was added 2-methyl-2-propanethiol (178 mi). The mixture was stirred at room temperature for 30 min, then 3-[1-(4-chlorobenzyl)-3-(t-butylthio)-5-methoxyindol-2-yl]-2,2-dimethylpropanoic acid methyl ester (150 g) (EP 419,049, Example 1, Step A) in DMF (450 mi) was added slowly. The mixture was slowly heated to 150° C. and kept at that temperature for 18 hours. After cooling to room temperature, the supernatant layer was decanted and the residue dissolved in H2O and acidifed with 1N HCl, extracted twice with Et2O, washed twice with brine, dried over MgSO4, filtered and evaporated to dryness to provide the title compound.

1. temperatureThe mixture was slowly heated to 150° C.
2. waitkept at that temperature for 18 hours
3. temperatureAfter cooling to room temperature
4. customthe supernatant layer was decanted
5. dissolutionthe residue dissolved in H2O
6. extractionacidifed with 1N HCl, extracted twice with Et2O
7. washwashed twice with brine
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. customevaporated to dryness