反应详情

温度

0 °C

124 ml of diisopropylamine is dissolved in 500 ml of THF under a blanket of dry nitrogen and cooled to 0° C. and 550 ml n-BuLi (1.6M in hexane) is added dropwise. Next, the mixture is cooled to minus 40° C., using an acetone/N2 bath, and 100 ml methyl 2-methylproponate is added. The resulting mixture is stirred for an additional 15 min at minus 40° C., after which 160.5 g of 3,4-dimethoxybenzoyl chloride dissolved in 750 ml of THF is added dropwise in 60 min during which the temperature is kept below −40° C. The cooling bath is removed and stirring is continued for 60 min at RT. 150 ml of 4M hydrochloric acid is added and the THF layer is separated and washed with 100 ml of water, 200 ml 1 M of sodium carbonate and 100 ml of brine, dried over MgSO4 and concentrated in vacuo.

1. temperatureNext, the mixture is cooled to minus 40° C.
2. additionis added dropwise in 60 min during which the temperature
3. customis kept below −40° C
4. customThe cooling bath is removed
5. stirringstirring
6. waitis continued for 60 min at RT
7. addition150 ml of 4M hydrochloric acid is added
8. customthe THF layer is separated
9. washwashed with 100 ml of water, 200 ml 1 M of sodium carbonate and 100 ml of brine
10. dry with materialdried over MgSO4
11. concentrationconcentrated in vacuo