반응 #216569

반응 방정식

water

N-(7-fluoro-4-propargyl-2H-1,4-benzoxazine-3(4H)-one-6-yl)-acetimidoylchloride

3,4,5,6-tetrahydrophthalamic acid monomethyl ester

triethylamine

→

N-acetyl-N-(7-fluoro-4-propargyl-2H-1,4-benzoxazine-3(4H)-one-6-yl)-3,4,5,6tetrahydrophthalamic acid methyl ester

용매

benzene

반응 조건

후처리

1. 1
   기타the reaction liquid stand
2. 2
   온도to cool the same, it
3. 3
   workup.ADDITIONwas poured
4. 4
   기타the organic layer was separated
5. 5
   세척The organic layer was washed first with water
6. 6
   건조with saturated brine, and then dried
7. 7
   농축The solvent was concentrated
8. 8
   workup.ADDITIONthe residue was treated by silica gel column chromatography (development solvent: ethyl acetate/n-hexane)

실험 절차

First, 0.44 g of N-(7-fluoro-4-propargyl-2H-1,4-benzoxazine-3(4H)-one-6-yl)-acetimidoylchloride and 0.29 g of 3,4,5,6-tetrahydrophthalamic acid monomethyl ester were dissolved in 15 ml of benzene, and 0.17 g of triethylamine was added to the solution at room temperature. After that the stirring was continued for 2 hr at 60° C. After letting the reaction liquid stand to cool the same, it was poured into cool water, and then the organic layer was separated therefrom. The organic layer was washed first with water and then with saturated brine, and then dried by using anhydrous magnesium sulfate. The solvent was concentrated, and then the residue was treated by silica gel column chromatography (development solvent: ethyl acetate/n-hexane) to obtain N-acetyl-N-(7-fluoro-4-propargyl-2H-1,4-benzoxazine-3(4H)-one-6-yl)-3,4,5,6tetrahydrophthalamic acid methyl ester. The melting point was 153°-154° C.

출처