反应详情

温度

110 °C

A solution of 500 mg (2.4 mmol) A3 in 5 ml dry dimethyl formamide under nitrogen was cooled in an ice bath and 73 mg (3.0 mmol) sodium hydride was added and the mixture was stirred for 10 minutes. After addition of 410 mg (2.6 mmol) ethyl bromoacetate, the mixture was heated to 110° C. for 8 h. The solvent was removed in vacuo and the residue was taken up in ethyl acetate and washed with water. The organic layer was dried over sodium sulphate and evaporated to dryness. Purification of the residue by column chromatography on SiGel (heptane/ethyl acetate 4:1) yielded 40 mg (6%) A15.

1. customThe solvent was removed in vacuo
2. washwashed with water
3. dry with materialThe organic layer was dried over sodium sulphate
4. customevaporated to dryness
5. customPurification of the residue by column chromatography on SiGel (heptane/ethyl acetate 4:1)
6. customyielded 40 mg (6%) A15