反应详情

A solution of 24-7 (360 mg, 1.17 mmol), 2-chloropyrimidine (145 mg, 1.26 mmol), and N,N-diisopropylethylamine (456 mg, 3.53 mmol) in ethanol (5 mL) was heated to 65° C. in a sealed tube (4 days). The solvent was removed in vacuo and the residue diluted in aqueous sodium carbonate and extracted with two portions of dichloromethane. The combined organics were washed with brine and dried (Na2SO4). The solvent was removed in vacuo. PCTLC (SiO2, 4mm, 1% NH4OEt; 10% EtOH; 90% CH2Cl2) afforded 24-8 (150 mg). ESLRMS m/e 386 g/mole (M++H, C21H31N5O2=386 g/mole.)

1. customThe solvent was removed in vacuo
2. additionthe residue diluted in aqueous sodium carbonate
3. extractionextracted with two portions of dichloromethane
4. washThe combined organics were washed with brine
5. dry with materialdried (Na2SO4)
6. customThe solvent was removed in vacuo