反应详情

温度

20 °C

HATU (1.1 g) was added in one portion to a cooled solution of 2-(3-(1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)methyl)-4-fluorophenyl)ethanol [Example 44, step c] (0.7 g) and 2-isopropylthiazole-4-carboxylic acid (0.39 g) and triethylamine (0.95 mL) in DMF (15 mL). The reaction mixture was stirred at 20° C. for 1 hour and then partitioned between ethyl acetate and brine. The organic layer was washed with brine (×2), dried, filtered and the solvent removed under reduced pressure. The crude product was purified by flash silica chromatography, using 3% methanol in ethyl acetate containing 1% triethylamine as solvent. Fractions containing the product were evaporated to dryness to afford the subtitled compound. Yield 0.61 g.

1. custompartitioned between ethyl acetate and brine
2. washThe organic layer was washed with brine (×2)
3. customdried
4. filtrationfiltered
5. customthe solvent removed under reduced pressure
6. customThe crude product was purified by flash silica chromatography
7. additionFractions containing the product
8. customwere evaporated to dryness