1-((氯甲氧基)甲基)-4-甲氧基苯

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: was prepared as described in Example 3 from chloromethyl 4-methoxybenzyl ether (see Preparation 4a and 4b) (10 mmol) and 5-chloropyrimidin-2-one (10 mmol) in 52% yield (1.45 g), m.p. 118° C. 1H NMR (CDCl3): δ3.77 (OMe), 4.57 (CH2Ph), 5.27 (CH2O), 6.6-7.3 (Ph), 7.63 and 8.35 (H-4, H-6, J 4 Hz). IR(KBr): 1670 cm1 (CO). was prepared

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred solution of diethyl 3,4-difluorophenylmalonate (13 g, 48 mmol) in dry tetrahydrofuran (100 ml) at 0° C. under a nitrogen atmosphere was added sodium hydride (1.5 g, 50 mmol) of 80% oil dispersion). The mixture was allowed to warm to room temperature and then heated to reflux for 1hour. To the cooled mixture was added 4-methoxybenzyl chloromethyl ether (9.5 g, 51 mmol ref. Synthesis, 1983, 762) and reflux was continued overnight. The cooled mixture was partitioned between water and diethyl ether, the organic layer was separated, dried over anhydrous magnesium sulphate and evaporated to leave diethyl 2-(3,4-difluorophenyl)-2(4-methoxybenzyloxymethyl)malonate as a yellow oil Nmr δ7.35 (1H,m), 7.2 (2H,d), 7.15-7.00 (2H,m), 6.85 (2H,d), 4.45 (2H,s), 4.20 (4H,q), 4.10 (2H,s), 3.80 (3H,s), 1.25 (6H,t). heated to reflux for 1hour reflux The cooled mixture was partitioned between water and diethyl ether the organic layer was separated dried over anhydrous magnesium sulphate evaporated