反应详情

To a stirred solution of 2-[(E)-2-(3-butyl-5-methyl-isoxazol-4-yl)-vinyl]-4-methyl-thiazole-5-carboxylic acid (200 mg, 0.65 mmol), 3,3-difluoroazetidine hydrochloride (93 mg, 0.72 mmol) and N-hydroxysuccinimide (86 mg, 0.74 mmol) in DMF (1 mL) was added 1-(3-dimethylaminopropyl)-3-ethylcarboiimide (144 mg, 0.75 mmol) and DMF (1 mL) followed by triethylamine (0.29 mL, 2.1 mmol) and DMF (2 mL). The resulting mixture was stirred under argon for 20 h and then water added and the mixture extracted with ethyl acetate. The combined organic extracts were dried, filtered and concentrated. Purification by chromatography (silica, 40% ethyl acetate in heptane) gave the title compound (73 mg, 29%) as pale yellow oil. MS: m/e=382.1 [M+H]+.

1. extractionthe mixture extracted with ethyl acetate
2. customThe combined organic extracts were dried
3. filtrationfiltered
4. concentrationconcentrated
5. customPurification by chromatography (silica, 40% ethyl acetate in heptane)