反应详情

A mixture of 4.0 g. of N-(4-chloro-3-hydroxyphenyl)-3,4,5,6-tetrahydrophthalimide, 4.7 g. of ethyl 2,3-dibromobutyrate, 2.4 g. of potassium carbonate and 35 ml. of acetone was refluxed with stirring for 6 hours and the precipitated salt was separated by a filtration. The filtrate was concentrated under a reduced pressure and 2N-HCl was added to the residue to obtain a crude crystal. The product was washed with water and dried and purified by a chromatography on a column of silica gel (developing solvent: ethyl acetate:n-hexane of 3:7) to obtain 5.2 g. of Compound No. 158 shown in Table 1.

1. additionA mixture of 4.0 g
2. customthe precipitated 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 obtain a crude crystal
6. washThe product was washed with water
7. customdried
8. custompurified by a chromatography on a column of silica gel (developing solvent: ethyl acetate:n-hexane of 3:7)
9. customto obtain 5.2 g