反应详情

温度

80 °C

A mixture of 8-(4-hydroxy-phenyl)-1,3-dipropyl-7-(2-trimethylsilanyl-ethoxymethyl)-3,7-dihydro-purine-2,6 dione (100 mg, 0.231 mmol), 4-methanesulfonyl methyl-pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester (82 mg, 0.254 mmol) and K2CO3 (63 mg, 0.462 mmol) in DMF (8 ml) was heated at 80° C. for 3 hrs. The reaction mixture was filtered through celite and washed with ethyl acetate. The filtrate was washed with water, brine, dried over sodium sulphate, filtered and concentrated under vacuum. The residue obtained was purified by column chromatography to offer 4-{4-[2,6-dioxo-1,3-dipropyl-7-(2-trimethylsilanyl-ethoxymethyl)-2,3,6,7-tetrahydro-1H-purin-8-yl]-phenoxymethyl}-pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester as a yellow oil (110 mg, 36%).

1. filtrationThe reaction mixture was filtered through celite
2. washwashed with ethyl acetate
3. washThe filtrate was washed with water, brine
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customThe residue obtained
8. customwas purified by column chromatography