反应详情

7-(2-Fluoro-4-iodo-phenylamino)-pyrrolo[1,2-c]pyrimidine-6-carboxylic acid (67 mg, 0.18 mmol), O-(2-vinyloxy-ethyl)-hydroxylamine (18 mg, 0.18 mmol), HOBt (26 mg, 0.19 mmol), EDCI hydrochloride (37 mg, 0.19 mmol) and DIPEA (31 μL, 0.18 mmol) were suspended in DMF (3 mL). The reaction mixture was stirred at room temperature for 16 hours, during which time the reagents dissolved. The reaction mixture was concentrated in vacuo, the resultant residue dissolved in ethyl acetate (10 mL), washed with aqueous saturated sodium bicarbonate solution (10 mL) and the aqueous fraction extracted twice with ethyl acetate (2×10 mL). The combined organic fractions were washed with brine, dried (MgSO4) and concentrated in vacuo. The resultant residue was subjected to flash chromatography (SiO2, gradient 0-100% ethylacetate in cyclohexane) to yield the title compound as a yellow solid (54 mg, 65%). LCMS (Method B): RT=3.38 min, M+H+=483.

1. dissolutiondissolved
2. concentrationThe reaction mixture was concentrated in vacuo
3. dissolutionthe resultant residue dissolved in ethyl acetate (10 mL)
4. washwashed with aqueous saturated sodium bicarbonate solution (10 mL)
5. extractionthe aqueous fraction extracted twice with ethyl acetate (2×10 mL)
6. washThe combined organic fractions were washed with brine
7. dry with materialdried (MgSO4)
8. concentrationconcentrated in vacuo