反应详情

温度

60 °C

A mixture of the product of Step B (0.34 g; 0.87 mmol) hydrochloride salt of tritylamine (0.22 g; 0.87 mmol) and N,N-diisopropylethylamine (DIPEA) (0.49 ml; 2.8 mmol) in anhydrous DMF (3 ml) was stirred for 2 h at 60° C. under N2. After removing the solvent in vacuo, the residue was diluted to 15 ml with ethyl acetate (EtOAc) and washed with, H2O, brine and dried over anhydrous MgSO4 and filtered. The filtrate was evaporated to dryness under reduced pressure and the residue was purified by FCC (SiO2; hexane/EtOAc, 8:2) to give pure title compound (0.2 g; 48%) as colourless heavy syrup. 1H-NMR (CDCl3) 3.86 (s, 2H); 3.87 (s, 2H); 6.81-7.57 (m, 18H).

1. customAfter removing the solvent in vacuo
2. additionthe residue was diluted to 15 ml with ethyl acetate (EtOAc)
3. washwashed with, H2O, brine
4. dry with materialdried over anhydrous MgSO4
5. filtrationfiltered
6. customThe filtrate was evaporated to dryness under reduced pressure
7. customthe residue was purified by FCC (SiO2; hexane/EtOAc, 8:2)