反应 #1211164
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07667053B2
反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 4-oxochromane-3-carboxylic acid, ethyl ester (4.0 g, 18 mmol) and 10% palladium on carbon (0.4 g) in 100 mL of acetic acid was degassed and filled with hydrogen using a balloon. After stirring at 70° C. overnight, the reaction mixture was filtered through CELITE diatomaceous earth, and the CELITE cake was washed with ethyl acetate (200 mL). The filtrate was washer with water (2×200 mL), dried over anhydrous sodium sulfate, filtered and concentrated to dryness to give the title compound. 1H NMR (500 MHz, CD3OD): δ 7.2-7.0 (m, 2H), 6.84 (t, 1H), 6.74 (d, 1H), 4.36 (dd, 1H), 4.21-4.13 (m, 3H), 3.03 (m, 3H), 1.26 (t, 3H). was degassed filled with hydrogen using a balloon the reaction mixture was filtered through CELITE diatomaceous earth the CELITE cake was washed with ethyl acetate (200 mL) dried over anhydrous sodium sulfate filtered concentrated to dryness
来源 ID: ord-1a58fc77b5cb46c293db5f2016ceaaf3