PREPARATION OF TRI-O-ALKYLCELLULOSES BY THE USE OF A NONAQUEOUS CELLULOSE SOLVENT AND THEIR PHYSICAL CHARACTERISTICS
PREPARATION OF TRI-O-ALKYLCELLULOSES BY THE USE OF A NONAQUEOUS CELLULOSE SOLVENT AND THEIR PHYSICAL CHARACTERISTICS
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DOI：
10.1002/app.1986.070310205
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发表时间：
1986-02-05
影响因子：
3
通讯作者：
NAKANO, J
中科院分区：
文献类型：
--
作者：
ISOGAI, A;ISHIZU, A;NAKANO, J
三-O-甲基-、-乙基-、-正丙基-、-正丁基-、-正戊基-、-异戊基-、-正己基-、-正庚基-、-正辛基-、-正癸基-和-3-苯氧基丙基-纤维素已经用粉末状氢氧化钠和相应的烷基碘或溴在一种非水纤维素溶剂SO2-二乙胺-二甲亚砜中制备。这些新的三-O-烷基纤维素通过红外光谱、13 C-NMR光谱和旋光度表征。上述前六种三-O-烷基纤维素以白色粉末形式获得，并且它们中的大多数（三-O-甲基-、-乙基-、-正丙基-和-正戊基-纤维素）由于近晶相或短沥青相而显示出热致液晶。另一方面，后五种衍生物即使在室温下也以胶状固体形式获得，并且由于choresteric相，在其浓氯仿溶液中容易显示溶致液晶。通过差示扫描量热法和X射线衍射分析对其中一些三-O-烷基-纤维素（三-O-甲基-、-乙基-、-正丙基-和-正丁基-纤维素）进行了表征。
Tri‐O‐methyl‐, ‐ethyl‐, ‐n‐propyl‐, ‐n‐butyl‐, ‐n‐pentyl‐, ‐iso‐amyl‐, ‐n‐hexyl‐, ‐n‐heptyl‐, ‐n‐octyl‐, ‐n‐decyl‐, and ‐3‐phenoxypropyl‐celluloses have been prepared with powdered sodium hydroxide and the corresponding alkyl iodides or bromides in one of nonaqueous cellulose solvents, SO2‐diethylamine‐dimethylsulfoxide. These new tri‐O‐alkylcelluloses were characterized by infrared spectra,13C‐NMR spectra, and optical rotations. The first six tri‐O‐alkylcelluloses described above were obtained as white powders and most of them (tri‐O‐methyl‐, ‐ethyl‐, ‐n‐propyl‐, and ‐n‐pentyl‐celluloses) showed thermotropic liquid crystals due to smetic or short pitch cholesteric phases. On the other hand, the latter five derivatives were obtained as gummy solids even at room temperature, and easily showed lyotropic liquid crystals in their concentrated chloroform solutions due to choresteric phases. some of these tri‐O‐alkyl‐celluloses (tri‐O‐methyl‐, ‐ethyl‐, ‐n‐propyl‐, and ‐n‐butyl‐celluloses) were characterized by differential scanning calorimetric and X‐ray diffractometric analyses.