RAFT试剂三硫代碳酸酯合成问题？第一次做，打算按照Macromolecules, Vol. 35, No. 18, 2002文献制作合成步骤：Synthesis of S,S'-Bis(R,R'-dimethyl-R''-acetic acid)-trithiocarbonate, 1. Carbon disulfide (27.4 g, 0.36 mol), chloroform (107.5 g, 0.9 mol), acetone (52.3 g, 0.9 mole), and tetrabutylammonium hydrogen sulfate (2.41 g, 7.1 mmol) were mixed with 120 mL of mineral spirits in a 1 L jacketed reactor cooled with tap water under nitrogen. Sodium hydroxide (50%) (201.6 g, 2.52 mol) was added dropwise over 90 min in order to keep the temperature below 25 °C. The reaction was stirred overnight. 900 mL of water was then added to dissolve the solid, followed by 120 mL of concentrated HCl (caution! gas, mercaptan odor) to acidify the aqueous layer. Stir for 30 min with nitrogen purge. Filter and rinse the solid thoroughly with water. Dry to constant weight to collect 41.3 g of earth-colored product. It can be further purified by stirring in toluene/acetone (4/1) or by recrystallizations from 60% 2-propanol or acetone to afford a yellow crystalline solid.我想问问mineral spirits究竟是什么？原料需要提纯么？反应需要一直在N2环境下么？小弟拜谢！查看更多7个回答 . 8人已关注
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