反应详情

A mixture of 15.0 g. of N-(4-bromo-3-hydroxyphenyl)-3,4,5,6-tetrahydrophthalimide, 12.0 g. of ethyl α-bromovalerate, 7.7 g. of potassium carbonate, 2.5 g. of potassium iodide and 50 ml. of acetone was refluxed with stirring for 3 hours and then, the reaction mixture was cooled to room temperature and the salt was separated by a filtration. The filtrate was concentrated under a reduced pressure and 2N-HCl was added to the residue to crystallize the product. The crystal was separated by a filtration and washed with water and dried. The residue was purified by a chromatography on a column of silica gel (developing solvent: ethyl acetate: n-hexane of 1:3) to obtain 17.6 g. of Compound No. 90 shown in table 1.

1. additionA mixture of 15.0 g
2. customthe salt was separated by a filtration
3. concentrationThe filtrate was concentrated under a reduced pressure and 2N-HCl
4. additionwas added to the residue
5. customto crystallize the product
6. customThe crystal was separated by a filtration
7. washwashed with water
8. customdried
9. customThe residue was purified by a chromatography on a column of silica gel (developing solvent: ethyl acetate: n-hexane of 1:3)
10. customto obtain 17.6 g