反应详情

温度

0 °C

DIAD (4.6 g, 0.029 mol) was added dropwise to a solution of methyl 3-hydroxy-5-{[phenylmethyl]oxy}benzoate (6 g, 0.023 mol), (S)-(+)-1-methoxy-2-propanol (2.59 g, 0.029 mol) and triphenylphosphine (7.53 g, 0.029 mol) in THF (100 mL), under argon, at 0° C. The reaction was stirred at 0° C. for 1 hour and at RT for 20 hours. The volatiles were removed in vacuo and isohexane/ethyl acetate 2:1 added followed by stirring for 1 hour. A white solid was removed by filtration and the filtrate was evaporated to a residue which was chromatographed on silica, eluting with a gradient of 0-20% ethyl acetate in isohexane, to give the desired compound (5.11 g).

1. customThe volatiles were removed in vacuo and isohexane/ethyl acetate 2:1
2. additionadded
3. stirringby stirring for 1 hour
4. customA white solid was removed by filtration
5. customthe filtrate was evaporated to a residue which
6. customwas chromatographed on silica
7. washeluting with a gradient of 0-20% ethyl acetate in isohexane