反应详情

A mixture of compound 2g [Compound of Formula 2 wherein R1=COOEt, R2, R3=(CH2)3] (10.0 g, 0.046 mol), ammonium acetate (3.64 g, 0.060 mol) and formic acid (35.74 mL, 0.946 mol) was stirred at 130-135° C. for 8 h. It was then cooled to room temperature and diluted with water (150 mL), extracted with ethyl acetate (3×100 mL), dried over Na2SO4, concentrated and purified by column chromatography to give pure compound of Formula (3g); 10.66 g; Yield: 97%; 1H NMR (200 MHz, CDCl3+DMSO-d6): δ 0.1.33 (t, J=8 Hz, 3H), 2.25-2.43 (m, 2H), 2.74-2.89 (m, 4H), 4.26 (q, J=8 Hz, 2H), 8.48 (s, 1H) 11.16 (bs, 1H).

1. extractionextracted with ethyl acetate (3×100 mL)
2. dry with materialdried over Na2SO4
3. concentrationconcentrated
4. custompurified by column chromatography