反应了102小时？

反应条件是合成羧酸环氧的，做醇肯定做不出，甚至那5%的纯度也难说

引用回帖:

2楼: Originally posted by 之之中人也 at 2017-12-27 21:11:43
反应了102小时？

Emrick的原文是反应了118小时，反应物就是我图片的反应物，原文如下：
17 (35.3 g, 249 mmol), triol 11 (10 g, 83 mmol),
and tetra-n-butylammonium chloride (3.45 mg,
12.5 mmol) were combined and stirred at 120 °C
as a homogeneous solution in a closed flask. The
mixture was stirred for 118 h at this temperature,
and the flask was removed from the heating bath.
The polymer product was dissolved in THF (20
mL) and fractionated into water (750 mL). The
water was decanted, and then the polymer was
dissolved in THF, dried over MgSO4, and concentrated in vacuo with stirring to obtain a viscous
liquid (27.2 g, 60%).
FTIR (n): 3380 (br, OH), 2934, 2859, 2409,
2290, 1460, 1365, 1106, 1053, 846 cm21. Mw
5 7300; Mn 5 2050; Mp 5 3100; PDI 5 3.5. Tg。请问反应时间太久还是？

引用回帖:

3楼: Originally posted by qilin112 at 2017-12-27 21:13:12
反应条件是合成羧酸环氧的，做醇肯定做不出，甚至那5%的纯度也难说

这个是原文中，使用我图片中的反应物的反应条件：17 (35.3 g, 249 mmol), triol 11 (10 g, 83 mmol),
and tetra-n-butylammonium chloride (3.45 mg,
12.5 mmol) were combined and stirred at 120 °C
as a homogeneous solution in a closed flask. The
mixture was stirred for 118 h at this temperature,
and the flask was removed from the heating bath.
The polymer product was dissolved in THF (20
mL) and fractionated into water (750 mL). The
water was decanted, and then the polymer was
dissolved in THF, dried over MgSO4, and concentrated in vacuo with stirring to obtain a viscous
liquid (27.2 g, 60%).
FTIR (n): 3380 (br, OH), 2934, 2859, 2409,
2290, 1460, 1365, 1106, 1053, 846 cm21. Mw
5 7300; Mn 5 2050; Mp 5 3100; PDI 5 3.5. Tg。请问这个反应条件又怎么成了羧酸环氧，不太懂，之前一直是做化工的
，

多元羧酸合成环氧树脂就是四丁基溴化铵，120度，但只需要几个小时。
羧酸的电离常数要比醇高几个数量级，所以这个反应几天，还是是有可能的，
但是如果体系中有水，因为水的电离常数比醇高，就会影响醇羟基的电离，建议原料除水，反应条件密闭除水，（ in a closed flask.）
你朋友说的有部分是对的，通氮气是一种简便的反应中防止水汽干扰的方法。

引用回帖:

6楼: Originally posted by qilin112 at 2017-12-27 21:57:59
多元羧酸合成环氧树脂就是四丁基溴化铵，120度，但只需要几个小时。
羧酸的电离常数要比醇高几个数量级，所以这个反应几天，还是是有可能的，
但是如果体系中有水，因为水的电离常数比醇高，就会影响醇羟基的电离 ...

那我可不可以参考文献方法，不通氮气，仅仅在一个除水的密封的环境下反应？毕竟通氮气，反应时间久了，晚上不太安全

有机强碱很容易开环环氧。所以呢，你最好每个小时监控环氧的环氧值，然后在做一个对比空白实验，研究四丁基氯化铵对环氧开环的影响！