反应详情

A solution of 5.0 g (35 mmol) of 1-methyl-(3-ethyl)-cyclobutanecarboxylic acid (prepared in Example 2A) in 35 ml of dry ether was stirred with ice-bath cooling under an argon atmosphere and 40 ml of a 2 M solution of methyllithuim in ether was added thereto. The resultant mixture was stirred without cooling for 3 hr. This mixture was then quenched by pouring the mixture into a vigorously stirred solution of 30 ml of methanol and 70 ml of water. The aqueous phase was separated and extracted twice with ether. The combined ether extract was dried over anhydrous magnesium sulfate and evaporated. The residue was distilled at reduced pressure to yield 2.5 g of the title compound having the following physical characteristics:

1. temperaturecooling under an argon atmosphere
2. temperaturewithout cooling for 3 hr
3. customThis mixture was then quenched
4. additionby pouring the mixture into a vigorously stirred solution of 30 ml of methanol and 70 ml of water
5. customThe aqueous phase was separated
6. extractionextracted twice with ether
7. extractionThe combined ether extract
8. dry with materialwas dried over anhydrous magnesium sulfate
9. customevaporated
10. distillationThe residue was distilled at reduced pressure