反应详情

温度

-40 °C

Trifluoroacetic acid anhydride (7.7 ml) was added dropwise to a solution of 5-bromovaleric acid (5 g) in tetrahydrofuran (25 ml) under nitrogen atmosphere at −40° C. and the solution was stirred at −40° C. for 30 minutes. To the mixture, was added tert-butanol (25 ml) at −40° C. and the stirring was continued for 3 hours while the temperature was gradually raised up to room temperature. Water and ethyl acetate were added to the mixture and the organic layer was separated, washed with a saturated sodium hydrogen carbonate aq. solution three times and then a saturated brine, dried over magnesium sulfate and concentrated in vacuo to give 5-bromovaleric acid tert-butyl ester (5.88 g). MS (m/z): 237/239 [M+H]+.

1. waitthe stirring was continued for 3 hours while the temperature
2. temperaturewas gradually raised up to room temperature
3. customthe organic layer was separated
4. washwashed with a saturated sodium hydrogen carbonate aq. solution three times
5. dry with materiala saturated brine, dried over magnesium sulfate
6. concentrationconcentrated in vacuo