Synthesis of gem-Dichlorocyclopropanes Using Liquid–Liquid Slug Flow,Bulletin of the Korean Chemical Society

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Synthesis of gem-Dichlorocyclopropanes Using Liquid–Liquid Slug Flow
Bulletin of the Korean Chemical Society ( IF 2.3 ) Pub Date : 2021-06-17 , DOI: 10.1002/bkcs.12346
Jong Won Lee ₁ , Yea Seul Jang ₁ , Jong Min Park ₁ , Chan Pil Park ₁

Affiliation

By analyzing the causes of precipitation and clogging in continuous flow dichlorocyclopropanation, we established that the flow reaction can be performed only with T-junctions and microtubes. Unlike tertiary amines, when quaternary ammonium salts were used as PTCs, precipitation and clogging in microchannels did not occur, and an excellent yield of up to 99% was obtained after optimizing the reaction temperature, reactant concentration, and retention time. In the scale-up experiment, the reaction yields slightly decreased as the inner diameter (ID) of the microchannel was increased, but the calculated throughput increased from 2.41 g/h (ID: 1.5 mm) to 3.46 g/h (ID: 1.9 mm) and 5.13 g/h (ID: 2.4 mm)

中文翻译：

使用液-液段塞流合成宝石-二氯环丙烷

通过分析连续流动二氯环丙烷反应中沉淀和堵塞的原因，我们确定流动反应只能用T形接头和微管进行。与叔胺不同，使用季铵盐作为PTC时，微通道中不会发生沉淀和堵塞，并且在优化反应温度、反应物浓度和保留时间后获得了高达99%的优异收率。在放大实验中，随着微通道内径 (ID) 的增加，反应产率略有下降，但计算出的吞吐量从 2.41 g/h (ID: 1.5 mm) 增加到 3.46 g/h (ID: 1.9)毫米）和 5.13 克/小时（内径：2.4 毫米）

更新日期：2021-08-19

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