反应详情

To methyl 2-(N-(2,4,6-trichlorophenyl)sulfamoylamino)acetate (3.0 g, 8.3 mmol), 2-methylpropan-1,3-diol (1.18 mL, 8.3 mmol) and PPh3 (5.4 g, 20.7 mmol), was dropwisely added DIAD (4 mL, 20.7 mmol) with adjustment of external temperature to 0° C. The reaction mixture was agitated for 3 hr at room temperature, extracted with EtOAc, dried (Na2SO4), filtered and concentrated under reduced pressure, followed by column chromatography (MeOH/DCM 1%), finally giving the title compound (2.3 g, y=65%, solid). 1H NMR (300 MHz, CDCl3): δ 7.41 (d, J=2.4 Hz, 1H), 7.37 (d, J=2.4 Hz, 1H), 4.44 (d, J=17 Hz, 1H), 4.37-3.86 (m, 5H), 3.59-3.41 (m, 1H), 3.38-3.13 (m, 1H), 2.75-2.53 (m, 1H), 1.32 (t, J=7.1 Hz, 3H), 0.94 (t, J=7.1 Hz, 3H).

1. customto 0° C
2. extractionextracted with EtOAc
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure