반응 #42764

반응 방정식

Water

2,4,6-trimethyl-benzenesulfonic acid 3-bromo-2-isopropyl-8-nitro-4-oxo-4H-chromen-7-yl ester

p-methoxybenzylamine

→

3-Bromo-2-isopropyl-7-(4-methoxybenzylamino)-8-nitro-chromen-4-one

용매

toluene

반응 조건

후처리

1. 1
   기타at 140° C. under microwave irradiation for a further 30 minutes
2. 2
   추출the mixture is extracted with ethyl acetate (3×100 ml)
3. 3
   세척washed with saturated brine (50 ml)
4. 4
   건조dried (MgSO4)
5. 5
   여과filtered
6. 6
   기타evaporated
7. 7
   기타The crude product is purified by chromatography on silica gel
8. 8
   기타The product-containing fractions are evaporated under reduced pressure
9. 9
   기타the residue is triturated with diethyl ether
10. 10
    기타to give a pale yellow solid

실험 절차

To a solution of 2,4,6-trimethyl-benzenesulfonic acid 3-bromo-2-isopropyl-8-nitro-4-oxo-4H-chromen-7-yl ester (1.906 g, 3.5 mmol) in dry toluene (18 ml) in a 20 ml capacity microwave tube is added p-methoxybenzylamine (0.69 ml, 5.26 mmol). The mixture is heated at 130° C. under microwave irradiation for 90 minutes and then at 140° C. under microwave irradiation for a further 30 minutes. Water (40 ml) is added, and the mixture is extracted with ethyl acetate (3×100 ml). The ethyl acetate extracts are combined, washed with saturated brine (50 ml), dried (MgSO4), filtered and evaporated. The crude product is purified by chromatography on silica gel using cyclohexane-ethyl acetate (8:1) as eluant. The product-containing fractions are evaporated under reduced pressure, and the residue is triturated with diethyl ether to give a pale yellow solid.

출처