99314-44-0 (3-甲基氧杂环丁烷-3-基)甲基4-甲基苯磺酸酯

常温运输。危险等级为IRRITANT（刺激性），海关编码2904100090，非危险化学品。

化学合成

化学合成

合成路线 1（1. 合成：99314-44-0）

• 产率：95%
• 合成条件：With 1-methyl-1H-imidazole; triethylamine In dichloromethane at 25℃; for 2 h;
• 实验步骤：1.向N-014-005_1（10g，97.9mmol）的DCM（100mL）溶液中加入1-甲基-1H-咪唑（16.0g，195mmol）和TEA（19.7g，195mmol）。25℃。将TsCl（37.1g，195mmol）加入到溶液中。将反应混合物在25℃下搅拌2小时。将混合物用水（2×100mL），盐水（100mL）洗涤，用Na₂SO₄干燥，过滤并在真空下浓缩，得到N-014-005_2（25g，粗品），为浅黄色固体，将其纯化。通过硅胶柱色谱法（0至15％EtOAc的PE溶液）得到N-014-005_2（23.6g，95％），为白色固体。1H NMR（400MHz，CDCl₃）δ7.80-7.68（m，2H），7.41-7.26（m，2H），3.40-3.29（m，4H），4.12-4.00（s，2H），2.44（s，3H），1.28（s，3H）。
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