反应详情

温度

20 °C

HATU (0.322 g) was added in one portion to a solution at 0° C. of tert-butyl 7-oxa-3,10-diazaspiro[5.6]dodecane-3-carboxylate (example 89, step e) (0.176 g) and 2-methylthiazole-4-carboxylic acid (0.093 g) and triethylamine (0.36 mL) in DMF (10 mL). The mixture was then stirred at 20° C. for 1 hour. The reaction mixture was partitioned between ethyl acetate and brine. The organic layer was washed twice with brine, dried over sodium sulphate, filtered and the solvent evaporated under reduced pressure. The crude product was purified by flash silica chromatography eluting with ethyl acetate. Pure fractions were evaporated to dryness to afford the subtitled compound. Yield 210 mg.

1. customThe reaction mixture was partitioned between ethyl acetate and brine
2. washThe organic layer was washed twice with brine
3. dry with materialdried over sodium sulphate
4. filtrationfiltered
5. customthe solvent evaporated under reduced pressure
6. customThe crude product was purified by flash silica chromatography
7. washeluting with ethyl acetate
8. customPure fractions were evaporated to dryness