9,9,- Bis(3,4-dihydroxyphenyl)fluorene synthesis

Yield:351521-78-3 85.1%

Reaction Conditions:

with 3-mercaptopropionic acid in chlorobenzene at 140; for 6 h;

Steps:

7 Example 7

3.6 g of 9-fluorenone, 8.8 g of o-diphenol, 3.8 g of activated clay catalyst, 0.2 g of 3-mercaptopropionic acid, 40 g of chlorobenzene were sequentially added to a three-necked flask equipped with a stirrer, a thermometer and a water separator (with a condenser); the stirring was started, and the reflux was heated (140°C). And the water is divided, the reaction is carried out for 6 hours, and the reaction is filtered while hot; the residue recovery is used for the next reaction after activation at 120 ° C; the filtrate is cooled to 0 ° C and then filtered for 1 hour to obtain a crude product.The filtrate is recovered and used in the next reaction of the product; The crude product obtained with toluene - acetone mixed solvent (volume ratio 1: 1) was recrystallized to give 9,9-bis (3,4-hydroxyphenyl) fluorene 6.5 g of a white solid, yield 85.1%, melting point measured It was 252.0 to 254.2 ° C, and the HPLC purity was 99.4%.

References:

CN108863728,2018,A Location in patent:Paragraph 0042; 0043