Simple and Efficient One-Step Synthesis of a Highly Enantioselective Catalyst 3,3-Di(pyrrolidinylmethyl)-H8BINOL
Simple and Efficient One-Step Synthesis of a Highly Enantioselective Catalyst 3,3-Di(pyrrolidinylmethyl)-H8BINOL
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简单高效的一步合成高对映选择性催化剂 3,3-二(吡咯烷基甲基)-H8BINOL
DOI：
10.1080/00397911.2015.1030032
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发表时间：
2015
影响因子：
2.1
通讯作者：
Pu Lin
中科院分区：
文献类型：
--
作者：
Gu Shuang-Xi;Huang Wen-Cai;Wu Xue-Dan;Ying Jun;Pu Lin
提出了一种简便的一步法合成(S)-3，3‘-二(吡咯烷甲基)-H_8BINOL。在最佳反应条件下，产品收率分别为83%(重结晶)和93%(柱层析)。该新工艺将吡咯烷/多聚甲醛/(S)-H8BINOL的摩尔比从58：58：1降低到3：3：1，将以前报道的两步反应简化为一步反应，不需要冷却和溶剂脱气等繁琐的操作，避免了大量含二恶烷的废水排放。
A concise one-step synthetic method was developed to prepare (S)-3,3′-di(pyrrolidinylmethyl)-H8BINOL via Mannich-type reaction. Under the optimal reaction conditions, the yield reached 83% (by recrystallization) and 93% (by column chromatography). This new procedure has reduced the molar ratio of pyrrolidine/paraformaldehyde/(S)-H8BINOL from 58:58:1 to 3:3:1, which simplified the previously reported two-step reaction to a one-step reaction with no need for laborious operations such as cooling and solvent degassing, and avoided discharging a large amount of dioxane-containing waste water.