Solvent-free microwave-assisted synthesis was carried out to prepare 2,3-dihydroxypropyl decanoate, by esterification of decanoic acid in the presence of two distinct glycerol derivatives, glycidol and glycerol carbonate, respectively. The process described is based on microwaves heating source with electrical power in the range of 200 W to 400 W, involving stoichiometric proportions of decanoic acid and glycerol derivatives, and using catalytic amounts of TBAI used as organocatalyst. Conversion and selectivity rates of esterification reactions were monitored by 1H and 13C{1H} NMR spectroscopy. The predominantly formed ester, 2,3-dihydroxypropyl decanoate was fully characterized by infrared and NMR spectroscopy, mass spectrometry and elemental analysis. Compared with the classical heating procedures, and whatever the glycerol derivatives used, total conversions were obtained with considerably reduced reaction times. Thus, under 300 W, esterification requires only one minute exposure from glycidol and five minutes from glycerol carbonate. The use of heating with conventional oil bath conditions needs residence times of more than one hour (even 24 hours in the case of glycerol carbonate). The microwave-assisted synthesis also notably enhances the selectivity in 2,3-dihydroxypropyl decanoate (at 300 W, 90 and 50 %, respectively), reinforcing the efficiency and the interest of the method. Practical applications: The results establish that microwave heating is well suited for the solvent-free synthesis of glycerol monodecanoate from decanoic acid and two glycerol derivatives, glycidol and glycerol carbonate. Reaction times are drastically reduced, and in both cases, marked improvements of the conversion and selectivity are recorded. The target α-monoglyceride, 2,3-dihydroxypropyl decanoate, has various potential applications such as antimicrobial properties, bacterial inhibitory activity, or denture disinfectant.

中文翻译：

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单癸酸甘油的高效微波辅助合成

在两种不同的甘油衍生物缩水甘油和甘油碳酸酯存在下，通过癸酸的酯化，进行无溶剂微波辅助合成以制备 2,3-二羟丙基癸酸酯。所描述的方法基于微波加热源，功率范围为 200 W 至 400 W，涉及化学计量比例的癸酸和甘油衍生物，并使用催化量的 TBAI 作为有机催化剂。酯化反应的转化率和选择性通过 1 H 和 13 C{1H} NMR 光谱监测。主要形成的酯，2,3-二羟丙基癸酸酯通过红外和核磁共振光谱、质谱和元素分析进行​​了充分表征。与经典的加热程序相比，无论使用何种甘油衍生物，反应时间显着缩短，获得了总转化率。因此，在 300 W 下，酯化只需要暴露于缩水甘油一分钟，暴露于甘油碳酸酯 5 分钟。在常规油浴条件下使用加热需要超过一小时的停留时间（在碳酸甘油的情况下甚至需要 24 小时）。微波辅助合成还显着提高了 2,3-二羟丙基癸酸酯的选择性（分别为 300 W、90% 和 50%），增强了该方法的效率和兴趣。实际应用：结果表明，微波加热非常适合从癸酸和两种甘油衍生物（缩水甘油和碳酸甘油酯）无溶剂合成单癸酸甘油酯。反应时间大大减少，在这两种情况下，记录了转化率和选择性的显着改善。目标α-单甘油酯，2,3-二羟丙基癸酸酯，具有多种潜在应用，例如抗菌特性、细菌抑制活性或义齿消毒剂。