PURIFICATION METHOD OF TRITYL GROUP-CONTAINING MONO-DISPERSED POLYETHYLENE GLYCOL

• Main Authors: TSUBUZAKI TAKUMA, YOSHIMURA KOHEI, OGI KOICHI
• Format: Patent
• Language: English; Japanese
• Published: 10.10.2019
• Subjects: CHEMISTRY; COMPOSITIONS BASED THEREON; MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONSONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS; METALLURGY; ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP

To provide a purification method for providing trityl group-containing mono-dispersed polyethylene glycol.SOLUTION: There is provided a purification method for separating and removing a ditrityl body from a mixture containing single-terminal trityl group-containing mono-dispersed polyethylene glycol and double-terminal ditrityl body impurities to obtain single-terminal trityl group-containing mono-dispersed polyethylene glycol, including Process (A): reacting a hydroxyl group of the trityl group-containing mono-dispersed polyethylene glycol with a dibasic acid anhydride in a solvent II, Process (B): separating the resulting reaction solution into a water layer and an organic layer by a separating extraction purification using one or more solvent selected from solvents I, II, III and a solution with pH 3 to 7, and distributing the ditrityl body impurities into the organic layer and an ester compound into the water layer, Process (C): adding base to the water layer to hydrolyze the ester compound to obtain the trityl group-containing mono-dispersed polyethylene glycol. Solvent I: C3 or less alcohol. Solvent II: C8 or less aromatic hydrocarbon. Solvent III: C10 or less saturated aliphatic hydrocarbon.SELECTED DRAWING: None 【課題】トリチル基含有単分散ポリエチレングリコールを得る精製方法。【解決手段】片末端トリチル基含有単分散ポリエチレングリコールおよび両末端ジトリチル体不純物を含む混合物から、ジトリチル体を分離除去し、片末端トリチル基含有単分散ポリエチレングリコールを得る精製方法で、工程（Ａ）：溶剤ＩＩ中で、トリチル基含有単分散ポリエチレングリコールの水酸基を二塩基酸無水物と反応。工程（Ｂ）：得られた反応溶液と、溶剤Ｉ、ＩＩ、ＩＩＩから選ばれた一種以上の溶剤とｐＨ3〜7の水溶液とを用いた分液抽出精製により水層と有機層とを分離し、ジトリチル体不純物を有機層に分配しエステル化合物を水層に分配。工程（Ｃ）：水層に塩基を添加しエステル化合物を加水分解し、トリチル基含有単分散ポリエチレングリコールを得る。溶剤Ｉ：Ｃ３以下のアルコール。溶剤ＩＩ：Ｃ8以下の芳香族炭化水素。溶剤ＩＩＩ：Ｃ10以下の飽和脂肪族炭化水素。【選択図】なし