反应 #2348141

反应方程式

Pentaerythritol

pyridine

DMF

1-O-(5,9,13,17-tetramethyloctadecanoyl)erythritol

methylene chloride

→

5,9,13,17-tetramethyloctadecanoic acid chloride

反应条件

后处理

1. 1
   workup.DISSOLUTIONdissolved
2. 2
   温度with heating

实验过程

Pentaerythritol (3.81 g), 2.21 g of pyridine, and 120 ml of dry DMF were mixed and dissolved with heating. The product was cooled to room temperature, the solution of 5 g of 5,9,13,17-tetramethyloctadecanoic acid chloride obtained in the step of synthesis of 1-O-(5,9,13,17-tetramethyloctadecanoyl)erythritol [formula (7)] in 5 ml of methylene chloride was added dropwise thereto, and the mixture was then agitated at room temperature for 1 hour. 100 ml of Methylene chloride was added to the resulting reaction solution, the mixture was washed 3 times with saturated saline, and dried over anhydrous sodium sulfate. Following filtration and concentration under reduced pressure, the concentrate was purified by silica gel column chromatography to obtain 2.50 g of mono-O-(5,9,13,17-tetramethyloctadecanoyl)pentaerythritol having the following properties. The purity determined by HPLC analysis was not lower than 99.5%. The results of NMR analysis are as shown below.

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