反应详情

Ethanol (8.72 mL, 150 mmol), DMAP (304 mg, 2 mmol), EDC (9.56 g, 50 mmol), and triethylamine (6.91 mL, 50 mmol) were added under cooling (ice) to a solution of (2-chloro-4-methoxy-phenyl)-acetic acid (10.00 g, 50 mmol, [CAS Reg. No. 91367-09-8]) in CH2Cl2 (200 mL). The reaction mixture was stirred at r.t. overnight, then diluted (CH2Cl2), and washed (1N aqueous HCl). The organic layer was dried (Na2SO4), and the solvent was evaporated. Purification of the residue by column chromatography (silica gel, heptane:ethyl acetate=100:0-70:30) gave the title compound (7.27 g, 64%). 1H NMR (300 MHz, CDCl3) 7.18 (1H, d), 6.94 (1H, d), 6.79 (1H, dd), 4.17 (2H, q), 3.79 (3H, s), 3.69 (2H, s), 1.26 (3H, t).

1. washwashed (1N aqueous HCl)
2. dry with materialThe organic layer was dried (Na2SO4)
3. customthe solvent was evaporated
4. customPurification of the residue by column chromatography (silica gel, heptane:ethyl acetate=100:0-70:30)