反应详情

温度

0 °C

To a reaction solution obtained by suspending 316 mg of potassium tert-butoxide in 18 ml of tetrahydrofuran (hereinafter abbreviated as THF) and cooling the suspension to 0° C. under a nitrogen stream was added a solution of 500 mg of the compound prepared in (1) above in 2 ml of THF, a bit at a time. After stirring for 10 minutes at the same temperature and an addition of 0.35 ml of butyl nitrite, the mixture was heated at 50° C. for 1 hour while stirring. Precipitates obtained by the addition of diethyl ether to the reaction mixture were collected by filtration. The powder thus obtained was suspended into a 10% aqueous solution of hydrochloric acid and extracted with ethyl acetate. The extract was washed with brine and dried over magnesium sulfate. The residue obtained by the concentration of the solvent was subjected to silica gel column chromatography using an ethyl acetate-hexane (1:1) mixed solvent as an eluant to obtain fractions containing the target compound. The fractions were concentrated to produce 320 mg of the title compound.

1. customTo a reaction solution obtained
2. temperaturethe mixture was heated at 50° C. for 1 hour
3. stirringwhile stirring
4. customPrecipitates
5. customobtained by the addition of diethyl ether to the reaction mixture
6. filtrationwere collected by filtration
7. customThe powder thus obtained
8. extractionextracted with ethyl acetate
9. washThe extract was washed with brine
10. dry with materialdried over magnesium sulfate
11. customThe residue obtained by the concentration of the solvent
12. additionmixed solvent as an eluant
13. customto obtain fractions
14. additioncontaining the target compound
15. concentrationThe fractions were concentrated