反应详情

温度

80 °C

To a solution of the product obtained in Step G (1.3 g) in DMF (134 ml) there are added 2,6-lutidine (4.15 ml) and 1,4-dibromo-butane (4.68 ml). The reaction mixture is stirred at 80° C. for 12 hours and at ambient temperature overnight. The reaction mixture is diluted with 600 ml of ethyl acetate. The organic phase is washed with saturated aqueous NaHCO3 solution, with water and with saturated aqueous NaCl solution, dried over magnesium sulphate, filtered and evaporated to dryness. The residue obtained is purified on silica gel (SiO2: gradient CH2Cl2/MeOH with the addition of 1.4N NH3 in the MeOH) to yield the title product, which is used directly in the next Step.

1. washThe organic phase is washed with saturated aqueous NaHCO3 solution, with water and with saturated aqueous NaCl solution
2. dry with materialdried over magnesium sulphate
3. filtrationfiltered
4. customevaporated to dryness
5. customThe residue obtained
6. customis purified on silica gel (SiO2
7. additiongradient CH2Cl2/MeOH with the addition of 1.4N NH3 in the MeOH)