反应详情

温度

100 °C

A solution of (S)-methyl 2-(3-(2,4-dimethoxybenzyl)ureido)-3-methylbutanoate (1.00 g, 3.10 mmol) in MeOH (7.5 mL) and NEt3 (0.430 mL, 3.10 mmol) in a sealed vessel was placed in preheated sand bath (at 100° C.) and heated for 18 hours. The cooled reaction mixture was concentrated and the residue was taken up in ether, washed with water, dried over sodium sulfate and filtered. Purification of the crude material by column chromatography, eluting with 1-3% MeOH/dichloromethane, afforded (S)-3-(2,4-dimethoxybenzyl)-5-isopropylimidazolidine-2,4-dione as an ivory colored solid (0.640 g, 71%). LCMS (APCI+) m/z 293 [M+H]+.

1. customThe cooled reaction mixture
2. concentrationwas concentrated
3. washwashed with water
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. customPurification of the crude material by column chromatography
7. washeluting with 1-3% MeOH/dichloromethane