反应详情

温度

2.5 °C

A stirred suspension of methyl 3-hydroxy-5-{[(2-methylphenyl)methyl]oxy}benzoate (15.3 g, 56.25 mmol) and triphenyl phosphine (14.4 g, 55 mmol) in dry chloromethane (900 ml) was cooled in an ice-bath and diisopropyl azodicarboxylate (11.88 ml, 55 mmol) was added dropwise. The reaction mixture was stirred at 0-5° C. for 30 minutes and (R)-methoxy-propan-2-ol was added dropwise. The reaction mixture was stirred at ambient temperature for 16 hours, and filtered through diatomaceous earth. The filtrate was evaporated and purified by column chromatograph on silica gel eluting with 10% ethyl acetate in iso-hexane to give the desired compound (10.7 g, 55%).

1. temperaturewas cooled in an ice-bath
2. stirringThe reaction mixture was stirred at ambient temperature for 16 hours
3. filtrationfiltered through diatomaceous earth
4. customThe filtrate was evaporated
5. custompurified by column chromatograph on silica gel eluting with 10% ethyl acetate in iso-hexane