反应详情

A solution of 3'-(m-trifluoromethylphenyl)-spiro[isobenzofuran-1(3H),5'(4'H)-isoxazol]-3-one (10 g., 0.03 mole) and concentrated H2SO4 (1 ml.) in n-pentyl alcohol (150 ml.) was held at reflux for 14 hours, cooled and poured into 300 ml. of ice water. The mixture was extracted with 600 ml. of ether. The ethereal solution was washed two times with water, dried over CaSO4 and concentrated under vacuum to give 12.05 g. of product as a yellow oil (99%). The oil was chromatographed on silica gel using ethyl acetate as the eluant. 8.4 g. of colorless oil was collected; ir (CHCl3) 1725 cm-1 ; nD25 =1.537.

1. temperatureat reflux for 14 hours
2. temperaturecooled
3. additionpoured into 300 ml
4. extractionThe mixture was extracted with 600 ml
5. washThe ethereal solution was washed two times with water
6. dry with materialdried over CaSO4
7. concentrationconcentrated under vacuum
8. customto give 12.05 g
9. customThe oil was chromatographed on silica gel
10. customof colorless oil was collected