反应详情

To a mixture containing methoxymethylamine hydrochloride (44 g, 0.45 mol) and triethylamine (138 mL, 0.99 mol) in CH2Cl2 (500 mL) at 0° C. was added over 30 min, 4-fluorobenzoyl chloride (50 mL, 0.41 mol). The result-ing mixture was allowed to warm to rt and stirring was continued for 30 min, at which time the mixture was poured into H2O and extracted with Et2O. The organic extract was washed with saturated aqueous NaCl and dried (MgSO4). Removal of the solvent in vacuo afforded the title compound (80 g, 100%), which was used without further purification: 1H NMR (CDCl3): d 7.72 (dd, 2H); 7.06 (apparent t, 2H); 3.52 (s, 3H); 3.43 (s, 3H).

1. additionwas added over 30 min
2. extractionextracted with Et2O
3. extractionThe organic extract
4. washwas washed with saturated aqueous NaCl
5. dry with materialdried (MgSO4)
6. customRemoval of the solvent in vacuo