反应详情

温度

105 °C

Compound 121 (16.12 g, 0.081 mol) was dissolved in 500 mL of DMF. Then 100 mL of methylene chloride and 26 g (0.464 mol) of potassium carbonate were added. The mixture was heated to 105° C. with vigorous stirring for 6 hours. The potassium carbonate was filtered and the DMF was removed in vacuo. The residue was poured into ice-water and let stand overnight. The precipitated product 122 was filtered and washed with water until neutral. The dried gray white solid weighed 15.60 g (yield 91%) and was recrystallized from methanol as brilliant long needles, m.p. 122°-124° C. IR cm-1 1710 (ester C=O); 1H NMR δ ppm 3.90 (s, 3H, OCH3), 3.95 (s, 3H, ArOCH3), 6.11 (s, 2H, OCH2O), 6.57 and 7.45 (each d, J=9 Hz, 1H, ArH). Anal. (C10H10O5)C, H.

1. filtrationThe potassium carbonate was filtered
2. customthe DMF was removed in vacuo
3. additionThe residue was poured into ice-water
4. waitlet stand overnight
5. filtrationThe precipitated product 122 was filtered
6. washwashed with water until neutral
7. customwas recrystallized from methanol as brilliant long needles, m.p. 122°-124° C