Triethylamine [121-44-8] M 101.2, b 89.4°, d 0.7280, n 1.4005, pK25 10.82.
Dried with
CaSO4, LiAlH4, Linde type 4A molecular sieves, CaH2, KOH, or K2CO3, then dis
td, either alone or from BaO,
sodium, ?2O5 or CaH2. It has also been distd from zinc dust, under nitrogen.
To remove traces of primary and
secondary amines, triethylamine has been refluxed with acetic anhydride, ben
zoic anhydride, phthalic anhydride,
then distd, refluxed with CaH2 (ammonia-free) or KOH (or dried with activate
d alumina), and again distd.
Another purification involved refluxing for 2h with /7-toluenesulfonyl chlor
ide, then distd. Grovenstein and
Williams [J Am Chem Soc 83 412 1961] treated triethylamine (50OmL) with benz
oyl chloride (3OmL), filtered
off the ppte, and refluxed the liquid for Ih with a further 3OmL of benzoyl
chloride. After cooling, the liquid
was filtered, distd, and allowed to stand for several hours with KOH pellets
. It was then refluxed with, and distd
from, stirred molten potassium. Triethylamine has been converted to its hydr
ochloride, crystd from EtOH (to m
254°), then liberated with aq NaOH, dried with solid KOH and distd from sod
ium under nitrogen.

【 在 tofindanID.bbs@bbs.nankai.edu.cn (C h a n g e d) 的大作中提到: 】
: 至少应该先蒸出来再进行第二步处理
: 否则体系中的H2O还是存在的
: 只是被KOH暂时吸收
: ...................
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FROM 202.112.26.*