反应详情

HATU (0.35 g) was added to a colourless solution of 2-(3-(1-oxa-4,9-diazaspiro[5.5]undecan-9-ylmethyl)-2-fluorophenyl)ethanol [Example 9, step b] (0.364 g), 2-(pentan-3-yl)thiazole-4-carboxylic acid [Carboxylic Acid 3] (0.141 g) and triethylamine (0.30 mL) in DMF (10 mL), pre-cooled in ice-water. The resulting yellow mixture was stirred in ice-water for 1 hour, then at room temperature for 1 hour. The solution was poured into a mixture of water and brine and extracted twice with ethyl acetate. The combined organic extracts were washed three times with water, once with brine, then dried (MgSO4), filtered and concentrated onto flash silica in vacuo. The resulting powder was purified by flash chromatography on silica eluted with triethylamine:methanol:dichloromethane (1:2:97) to afford the subtitled compound. Yield 0.324 g.

1. extractionextracted twice with ethyl acetate
2. washThe combined organic extracts were washed three times with water
3. dry with materialonce with brine, then dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated onto flash silica in vacuo
6. customThe resulting powder was purified by flash chromatography on silica
7. washeluted with triethylamine:methanol:dichloromethane (1:2:97)