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With sodium bromide; In acetone; for 30h;Heating / reflux;Product distribution / selectivity;
25 g (97.53 mmol) of toluene-4-sulfonic acid 3-methyl-oxetane-3-yl methyl ester synthesized according to Synthesis Example 1 and 50.18 g (0.49 mol) of NaBr were added to 250 ml of acetone, and the mixture was stirred under reflux for 30 hours. The obtained precipitate was filtered, and the mixture was observed until the mixture become colorless by adding charcoal. The charcoal was filtered and the solvent was removed under reduced pressure to obtain 14.8 g of 3-methyl-3-(bromomethyl)oxetane (Yield: 92%). NMR spectroscopy of the resulting product was: 1H NMR (CDCl3, 300MHz): delta4.46-4.38 (d+d, 4H), 3.65(s, 2H), 1.44(s, 3H).
With lithium bromide; In acetone; at 65℃; for 1h;
2. To a solution of N-014-005_2 (10 g, 39.0 mmol) in acetone (100 mL) was added LiBr (13.5 g, 156 mmol). The mixture was stirred at 65C for 1 hrs. The mixture was quenched with water (200 mL) at 0C and extracted with hexane (3 x 200 mL). The combined organic phase was washed with brine (50 mL), dried over Na2SO4, filtered and concentrated to give N-014-005_3 (2.54 g, crude) as yellow liquid. 1H NMR (400 MHz, CDCl3) delta 4.50-4.30 (m, 4H), 3.64 (s, 2H), 1.58 (s, 1H), 1.43 (s, 3H).
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