反应详情

To a slurry of 26.4 mg. (1.1 mmoles) of sodium hydride in 2 ml. of benzene was added 231 mg. (1 mmole) of 2,2-dimethyl-5-ethyl-6-oxo-2,3,6,7-tetrahydro-furo[2,3-f]indole and the resultant reaction mixture stirred for 5 minutes. To the reaction mixture was added 0.13 ml. (1.1 mmoles) of diethyl carbonate, and the mixture allowed to stir 18 hours. The reaction is then added to methylene chloride and 4N hydrochloric acid, and the organic phase separated, washed with water and a saturated brine solution and dried over magnesium sulfate. The extract was subsequently treated with 1N sodium hydroxide solution and the basic layer separated. The aqueous basic layer was acidified and the product extracted with methylene chloride. The organic phase was separated, dried with magnesium sulfate and concentrated to give 155 mg. (51% yield) of the titled intermediate as an oil.

1. additionTo the reaction mixture was added 0.13 ml
2. stirringto stir 18 hours
3. customthe organic phase separated
4. washwashed with water
5. dry with materiala saturated brine solution and dried over magnesium sulfate
6. additionThe extract was subsequently treated with 1N sodium hydroxide solution
7. customthe basic layer separated
8. extractionthe product extracted with methylene chloride
9. customThe organic phase was separated
10. dry with materialdried with magnesium sulfate
11. concentrationconcentrated
12. customto give 155 mg