反应详情

温度

65 °C

To a stirred solution of methyl 3-(benzyloxy)-2,2-dimethylpropanoate prepared according to Step A (952 mg, 4.28 mmol), in THF (11 mL) was added aqueous 1M NaOH (5.14 mL, 5.14 mmol). Little to no progress was seen at ambient temperature. Additional NaOH (˜7 mL, ˜7 mmol) was then added and the temperature was raised to 65° C., for 20 hours. After cooling to ambient temperature, the bulk of the THF was removed in vacuo. Aqueous 3M HCl (˜5 mL, ˜15 mmol) was then slowly added, resulting in the formation of a precipitate. This mixture was filtered through filter paper, and washed with a minimal amount of water. After placing under a strong vacuum for a few hours, the title compound was obtained. MS: m/z=231 (M+23 (Na+)).

1. customwas seen at ambient temperature
2. temperatureAfter cooling to ambient temperature
3. customthe bulk of the THF was removed in vacuo
4. customresulting in the formation of a precipitate
5. filtrationThis mixture was filtered
6. filtrationthrough filter paper
7. washwashed with a minimal amount of water
8. waitAfter placing under a strong vacuum for a few hours