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发表于 2012-11-11 05:44:36 来自手机 |显示全部楼层

碘甲烷甲基化

本帖最后由 九月风 于 2012-11-11 19:49 编辑

是不是碘甲烷就可以呀!二楼用的甲醛,我换成碘甲烷还以他的化合物为底物
反应步骤 :To a round-bottom flask were added NaH (0.782 g, 19.5 mmol, prewashed with dry hexane) and dry THF (45 ml). To the round-bottom flask was added (R)-phenylethyl amine (18.2 mmol,2.20 g, 2.35 ml) in dry THF (37 ml). The solution was stirred over night. Methyl iodide (18.2 mmol, 2.63 g, 1.16 ml) in dry THF (23 ml) was added dropwise over 2 h. The solution was stirred for 8 h. The reaction was quenched with ice cold brine (100 ml) and extracted with diethyl ether (4×25 ml). The combined organic phases were dried over Na2SO4. Evaporation in vacuo
gave a light yellow oil which was distilled (bp 86°C/20 mmHg) at reduced pressure using a vigreux to yield 3b (2.14 g, 87%) as a colorless oil (>99% NMR).
Reference  from   Solid-phase supported chiral lithium amides used in deprotonation reactionsFull TextBy Johansson, Anna et al From Tetrahedron: Asymmetry, 14(10), 1261-1266; 2003

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