反应详情

A solution of (S)-tert-butyl 4-(1-cyano-2-(4-(1-methyl-2-oxoindolin-6-yl)phenyl)ethylcarbamoyl)tetrahydro-2H-pyran-4-ylcarbamate (Example 21, step (ii), 35 mg) in formic acid (5 mL) was stirred at 50° C. for 30 min. The reaction mixture was poured into ice/water (50 mL) and basified to pH 8 with 0.880 aqueous ammonia solution. The mixture was extracted with ethyl acetate (2×40 mL) and the organics were dried over sodium sulfate and evaporated in vacuo. The crude product was purified by reversed phase HPLC on a Waters' Sunfire column using methanol and aqueous 0.1% trifluoroacetic acid as eluent. The fractions containing the desired compound were evaporated to dryness to afford product which was further purified by chromatography on silica eluting with 3% 2M methanolic ammonia in dichloromethane. Pure fractions were evaporated to dryness to afford the titled compound (10 mg).

1. extractionThe mixture was extracted with ethyl acetate (2×40 mL)
2. dry with materialthe organics were dried over sodium sulfate
3. customevaporated in vacuo
4. customThe crude product was purified by reversed phase HPLC on a Waters' Sunfire column
5. additionThe fractions containing the desired compound
6. customwere evaporated to dryness
7. customto afford product which
8. customwas further purified by chromatography on silica eluting with 3% 2M methanolic ammonia in dichloromethane
9. customPure fractions were evaporated to dryness