反应详情

温度

90 °C

1.76 g of NH4Cl dissolved in 21 ml of water are added to a mixture heated to 90° C. of 7.0 g of the compound obtained in Step 4.1, and 4.44 g of Fe(0) in 400 ml of isopropanol and 100 ml of THF. The reaction mixture is heated for 4 hours at 90° C. A further 0.88 g of NH4Cl is added and the mixture is heated for 2 hours at 90° C. The resulting mixture is filtered while hot and the filtrate is evaporated under reduced pressure. The residue is taken up in EtOAc and washed twice with saturated NaHCO3 solution. The organic phase is dried over MgSO4 and filtered, and the filtrate is evaporated under reduced pressure. The residue is chromatographed on silica gel, eluting with a PE/EtOAc mixture from (100/0, v/v) to (40/60, v/v) to give 5.2 g of the expected product.

1. additionare added to a mixture
2. temperaturethe mixture is heated for 2 hours at 90° C
3. filtrationThe resulting mixture is filtered while hot and the filtrate
4. customis evaporated under reduced pressure
5. washwashed twice with saturated NaHCO3 solution
6. dry with materialThe organic phase is dried over MgSO4
7. filtrationfiltered
8. customthe filtrate is evaporated under reduced pressure
9. customThe residue is chromatographed on silica gel
10. washeluting with a PE/EtOAc mixture from (100/0