反应详情

温度

0 °C

To 5 ml CH2Cl2 was added 1 g of triester 62 (2.4 mmol, 1 equiv) and 0.3 g triethylamine (2.9 mmol, 1.2 equiv.) The solution was cooled to 0° C. with an ice bath and 0.23 g acetyl chloride (2.9 mmol, 1.2 equiv) was added dropwise. The solution was stirred for a further 4 hours and allowed to warm slowly to room temperature. The solution was poured into a separating funnel and washed with 2×15 ml HCl (5% aqueous) and 1×15 ml concentrated NaCl. The solution was dried over Na2SO4 and the solvent was removed in vacuo. The residue was dissolved in minimal EtOAc and loaded onto a silica column, where it was purified by column chromatography with EtOAc and hexane (1:1) to give 0.79 g of a white solid in 72% yield.

1. temperatureto warm slowly to room temperature
2. additionThe solution was poured into a separating funnel
3. washwashed with 2×15 ml HCl (5% aqueous) and 1×15 ml concentrated NaCl
4. dry with materialThe solution was dried over Na2SO4
5. customthe solvent was removed in vacuo
6. dissolutionThe residue was dissolved in minimal EtOAc
7. customwas purified by column chromatography with EtOAc and hexane (1:1)