反应详情

To a solution of 4-methylpiperazine-1-carboxylic acid [4-(4-amino-2-fluorophenoxy)pyridin-2-yl]amide (80 mg) in tetrahydrofuran (2.3 ml) was added a solution of phenylacetyl isocyanate in hexane (1.4 ml, Production Example 1), followed by stirring under a nitrogen atmosphere at room temperature for 2 hrs. The reaction mixture was partitioned between ethyl acetate (100 ml) and a saturated aqueous solution of sodium hydrogencarbonate (50 ml). The organic layer was dried over anhydrous sodium sulfate, and concentrated under a reduced pressure. The residue was purified by silica gel column chromatography (FUJI Silysia NH, eluent; hexane:ethyl acetate=1:1, ethyl acetate, then ethyl acetate:methanol=10:1). Fractions containing the target compound were concentrated to give a crude product, to which diethyl ether was then added to precipitate a solid. The solid was filtered off, washed with diethyl ether, and dried under aeration to provide the titled compound (55.2 mg, 47%) as colorless powder.

1. customThe reaction mixture was partitioned between ethyl acetate (100 ml)
2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
3. concentrationconcentrated under a reduced pressure
4. customThe residue was purified by silica gel column chromatography (FUJI Silysia NH, eluent
5. additionFractions containing the target compound
6. concentrationwere concentrated
7. customto give a crude product
8. customto precipitate a solid
9. filtrationThe solid was filtered off
10. washwashed with diethyl ether
11. customdried under aeration