反应详情

To a stirred suspension of (3-{5-[(2,4-dimethoxy-benzyl)-methyl-amino]-3H-isobenzofuran-1-ylidene}-6-fluoro-1,3-dihydro-indol-2-one (197 mg, 0.44 mmol) in methylene chloride (10 ml) was added trifluoroacetic acid (1 ml). The mixture was stirred for 30 minutes at room temperature and then evaporated to give a residue. The residue was treated with 50% MeOH in water (25 ml, containing 1 ml of triethylamine) with heating for 30 minutes. After filtered and dried under vacuum, the resulting solid was mixed with acetone (50 ml), and heated at 50° C. for 30 minutes. The mixture was cooled to room temperature and filtered. The filtrate solution was concentrated under reduced pressure to give a crude product. Trituration of the crude product with CHCl3/hexanes afforded 6-fluoro-3-(5-methylamino-3H-isobenzofuran-1-ylidene)-1,3-dihydro-indol-2-one as a yellow solid (100 mg, 76%).

1. customevaporated
2. customto give a residue
3. temperaturewith heating for 30 minutes
4. filtrationAfter filtered
5. customdried under vacuum
6. additionthe resulting solid was mixed with acetone (50 ml)
7. temperatureheated at 50° C. for 30 minutes
8. temperatureThe mixture was cooled to room temperature
9. filtrationfiltered
10. concentrationThe filtrate solution was concentrated under reduced pressure
11. customto give a crude product