反应详情

A mixture of 6 g of sodium salt of 5-(benzyloxy)-2-({1-[(1,1-dimethylethoxy)carbonyl]piperidin-4-yl}[(2-methylpropoxy)carbonyl]amino)benzoic acid obtained in stage 1.3 and 4.42 g of DIEA in 250 ml of DMF is stirred at AT for 15 min. 6.48 g of HBTU are added and the mixture is left stirring for 30 min. 2.48 g of veratrylamine are added and the reaction mixture is stirred for 48 h 00. It is evaporated under reduced pressure, the residue is taken up in AcOEt, washed with a saturated NH4Cl solution and with a saturated NaHCO3 solution, dried over Na2SO4 and filtered, and the solvent is evaporated under reduced pressure. The residue is chromatographed on silica gel, elution being carried out with an AcOEt/heptane mixture, (20/80, v/v) as far as (60/40, v/v), to give 7.5 g of expected product.

1. waitthe mixture is left
2. stirringstirring for 30 min
3. stirringthe reaction mixture is stirred for 48 h 00
4. customIt is evaporated under reduced pressure
5. washwashed with a saturated NH4Cl solution and with a saturated NaHCO3 solution
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. customthe solvent is evaporated under reduced pressure
9. customThe residue is chromatographed on silica gel, elution