Method for preparing 9-fluorenyl methanol

Abstract

The invention discloses a preparing method of 9-fluorene carbinol, which comprises the following steps: step 1. synthesizing 9-fluorene carbinol; step 11. sloughing one hydrogen of 9 position fluorene at proton pattern to generate fluorene positive ion to react with ethyl formate to obtain 9-fluorene formaldehyde; step 12. reducing 9-fluorene formaldehyde into coarse product of 9-fluorene carbinol; step 2. extracting the coarse product of 9-fluorene carbinol twice.

Description

technical field [0001] The invention relates to a method for preparing 9-fluorenemethanol, in particular to a method for synthesizing 9-fluorenemethanol from fluorene. Background technique [0002] 9-Fluorenemethanol is the raw material for the preparation of peptide FMOC series protective agents. Its application in the field of biomedicine is becoming more and more extensive, and the demand is increasing; and fluorene is a main component in coal tar, and its content in coal tar is 1 %~2%. my country has abundant fluorene resources, therefore, it is of great significance to use cheap fluorene to produce high value-added 9-fluorenemethanol. [0003] There are currently two methods for synthesizing 9-fluorenemethanol from fluorene, which are one-step synthesis method and two-step synthesis method. [0004] Described one-step synthetic method, it is by the scientist of Japan and Canada respectively take saturated hydrocarbon and tetrahydrofuran as solvent, take n-butyllithium...

AI Technical Summary

Problems solved by technology

[0008] 1. The strong base catalyst NaH will generate flammable hydrogen gas during the reaction process, which has a large safety hazard in the production process; while sodium ethoxide needs to be prepared on site before the reaction, and the process is complicated, otherwise its activity will be affected, resulting in a reaction yield. decline;

[0009] 2. The solvents ether and ethyl formate have low boiling points, 34.6°C and 53°C respectively, which cause a large amount of volatilization loss during use, which may easily cause safety accidents such as fire and explosion; a major safety hazard;

[0010] 3. The 9-fluorenemethanol produced by the reaction is generally purified by solvent recrystallization. The solvents used include ethanol, ether, petroleum ether, etc., which have limited ability to remove impurities and are difficult to meet the requirements of high purity.