反应详情

温度

20 °C

HATU (0.792 g) was added in one portion to a stirred solution at 0° C. of 2-(3-(2-(5-oxa-2,8-diazaspiro[3.5]nonan-2-yl)ethyl)phenyl)ethanol 2HCl (0.56 g) (example 176 step e), 2-isopropylthiazole-4-carboxylic acid (0.275 g) and triethylamine (1.117 ml) in DMF (7 mL). The mixture was stirred at 20° C. for 3 hours and then partitioned between ethyl acetate and brine, the organic layer was washed with brine (×2), dried, filtered and the solvent evaporated under reduced pressure. The crude product was purified by flash silica chromatography, 5% methanol in ethyl acetate with 1% triethylamine. Pure fractions were evaporated to dryness to afford the subtitled compound. Yield 0.475 g

1. custompartitioned between ethyl acetate and brine
2. washthe organic layer was washed with brine (×2)
3. customdried
4. filtrationfiltered
5. customthe solvent evaporated under reduced pressure
6. customThe crude product was purified by flash silica chromatography, 5% methanol in ethyl acetate with 1% triethylamine
7. customPure fractions were evaporated to dryness