反应详情

A solution of (3) (1.5 g, 4.3 mmol) in diglyme was heated at 150° C. in a microwave reactor (Smith Creator, S00219) for 40 minutes. Solvent evaporated under vacuum in Genevac Evaporator at 80° C. for 3hours to give a brown solid. This was taken in dichloromethane (40 ml) and treated with trifluoroacetic acid at room temperature for 2 hours. Solvent evaporated to dryness under reduced pressure, crude taken in water, washed with DCM, aqueous layer basified with 1M NaOH solution and extracted with dichloromethane. Organic layer dried over Na2SO4 and evaporated under reduced pressure to give pale brown solid (300 mg); 1HNMR (CDCl3) 8.14–8.10 (m, 2H), 7.59–7.47 (m, 3H), 4.83 & 4.65 (d, J=5 Hz, 1H), 3.18–3.05 (2m, 1H), 2H), 1.05–0.97 (2Xt, J=7.2 Hz, 3H).

1. customSolvent evaporated under vacuum in Genevac Evaporator at 80° C. for 3hours
2. customto give a brown solid
3. customSolvent evaporated to dryness under reduced pressure, crude
4. washwashed with DCM, aqueous layer
5. extractionextracted with dichloromethane
6. dry with materialOrganic layer dried over Na2SO4
7. customevaporated under reduced pressure