反应详情

温度

150 °C

A solution of 24-4 (1.00 g, 2.98 mmol) in triethyl orthoacetate (50 mL) was treated with propionic acid (2.5 mg, 0.034 mmol) and heated to 150 ° C. for 3 h. The reaction mixture was cooled to room temperature and treated with 1 N HCl and brine (75 mL each). The mixture was extracted with two portions of ethyl acetate. The combined organics were washed with brine and dried (Na2SO4). Purification via PCTLC (SiO2, 4 mm, 10% EtOH; 90% CH2Cl2) afforded 24-5 (650 mg).

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionThe mixture was extracted with two portions of ethyl acetate
3. washThe combined organics were washed with brine
4. dry with materialdried (Na2SO4)
5. customPurification via PCTLC (SiO2, 4 mm, 10% EtOH; 90% CH2Cl2)