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[求助]
求助己内酯与炔丙醇的开环反应
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最近在做己内酯与含有一元炔基的醇的开环反应，异辛酸亚锡为催化剂，甲苯为溶剂（已减压蒸馏），己内酯经减压蒸馏，反应前抽真空-通氮气循环三次，可是做了个红外还是没有发现炔基的伸缩振动峰，请问各位虫虫有什么好的建议？大家做己内酯的开环是用本体聚合还是溶液聚合呢？万分感谢啦，急急~~~ [ Last edited by slcoco on 2012-5-14 at 15:14 ] |
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ostrich1853
铁杆木虫 (著名写手)
杂货铺
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【答案】应助回帖
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Synthesis of a-Propargyl, x-Acetyl Terminated PCL The a-propargyl terminated PCL was prepared by ROP of CL in toluene with Sn(Oct)2 as a catalyst and propargyl alcohol as an initiator. CL (2.85 g, 25 mmol), propargyl alcohol (0.056 g, 1.0 mmol), Sn(Oct)2 (0.05 g, 0.125 mmol), and 30 mL of toluene were added into a glass tube. The mixture in the tube was degassed by three freeze-vacuumthaw cycles. The flask was then placed in an oil bath thermostated at 110 C for 24 h. After the polymerization, the polymer solution was cooled to room temperature and added into an excess of methanol. The precipitate was filtered off and dried at room temperature in a vacuum oven for 48 h. The resultant (CHBCCH2)PCL(OH) was dissolved in chloroform (2.0%, w/v) and then react with acetic anhydride (1.0%, v/v in chloroform) at room temperature for 24 h. The polymer formed was precipitated in methanol and then collected by filtration. After drying at room temperature in a vacuum oven for 48 h, the a-propargyl, x-acetyl terminated PCL, (CHBCCH2)PCL(OOCCH3) were obtained in 88% yield. 1H NMR (300 MHz, CDCl3), d (TMS, ppm): 4.67 (CHBCCH2OOC), 4.06 (CH2CH2CH2CH2 CH2OOC), 2.47 (CHBCCH2OOC), 2.30 (C(O) CH2CH2CH2), 2.02 (OOCCH3), 1.60 (CH2CH2CH2 CH2CH2), 1.32 (CH2CH2CH2CH2CH2). Mn(GPC) ¼ 3740; Mw/Mn ¼ 1.20. IR (KBr, cm1): 3438, 3269, 2946, 2859, 2123, 1733, 1645, 1468, 1419, 1374, 1299, 1249, 1192, 1108, 1047, 965,725. |
6楼2012-05-14 17:16:42
ostrich1853
铁杆木虫 (著名写手)
杂货铺
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2楼2012-05-14 15:25:34
3楼2012-05-14 16:31:54
ostrich1853
铁杆木虫 (著名写手)
杂货铺
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- 专业: 高分子合成化学
4楼2012-05-14 16:56:00