反应详情

温度

20 °C

A solution of 2-isopropylthiazole-4-carboxylic acid (1 g) and tert-butyl 1-oxa-4,9-diazaspiro[5.5]undecane-9-carboxylate hydrochloride (WuXi PharmaTech) (1.71 g) in DMF (30 mL) was cooled in an ice bath and treated with triethylamine (2.442 mL) followed by HATU (2.89 g). The ice bath was removed and the mixture was stirred at 20° C. for 1 hour. The 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 using 70% ethyl acetate in isohexane as solvent. Pure fractions were evaporated to dryness to afford the subtitled compound. Yield 2 g.

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