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HRID78963

反应详情

EQUATION

反应方程式

HRID 78963 的结构方程式

REACTANTS

反应物

2
结构：Cc1ccccc1O
HCID335

o-Cresol

C7H8O

结构：O=C1C=CC=C2C1=Cc1ccccc12
HCID22281833

未命名化合物

PRODUCTS

生成物

1
结构：Cc1cc(C2(c3ccc(O)c(C)c3)c3ccccc3-c3ccccc32)ccc1O
HCID11014345

4,4'-(9H-Fluorene-9,9-diyl)bis(2-methylphenol)

C27H22O2

收率 83.5%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：O.O=P(O)(O)O.[O]=[W](=[O])=[O].[O]=[W](=[O])=[O].[O]=[W](=[O])=[O].[O]=[W](=[O])=[O].[O]=[W](=[O])=[O].[O]=[W](=[O])=[O].[O]=[W](=[O])=[O].[O]=[W](=[O])=[O].[O]=[W](=[O])=[O].[O]=[W](=[O])=[O].[O]=[W](=[O])=[O].[O]=[W](=[O])=[O]
催化剂HCID16212977

Phosphoric acid--trioxotungsten--water (1/12/1)

H5O41PW12

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A reaction was carried out by (a) feeding 23 g of fluorenone, 0.57 g of tungstophosphoric acid, and 161 g of 2-methyl phenol into a 500 ml glass reactor vessel equipped with a stirrer, a condenser and a thermometer, and (b) stirring a mixture under a reduced pressure of 1.3×103 Pa at 70° C. for 4 hours while removing generated water out of the system. The amount of remaining fluorenone was determined by HPLC, and found to be 0.1% or less. To an obtained reaction mixture liquid, 0.6 g of 29% sodium hydroxide aqueous solution was added, and 103.5 g of 2-methyl phenol was recovered from an organic phase by concentration under reduced pressure. To a concentrated liquid, 161 g of toluene and 46 g of water were added, and the mixture liquid was stirred at 80° C. Thereafter, an aqueous phase was separated and removed, and a target substance partitioned in an organic phase was recovered. The organic phase was further washed twice with 46 g of water, and cooled to 10° C. Then, precipitated crystals were subjected to filtration and drying to obtain 40.3 g of 9,9-bis(4-hydroxy-3-methylphenyl)fluorene (yield: 83.5%, LC purity: 99.3%). Obtained 9,9-bis(4-hydroxy-3-methylphenyl)fluorene was dissolved by heat at 230° C. for 2 hours. The 9,9-bis(4-hydroxy-3-methylphenyl)fluorene thus dissolved show a hue of 1 or less in Gardner. The total amount of toluene used was 4 parts by weight relative to 1 part by weight of the 9,9-bis(4-hydroxy-3-methylphenyl)fluorene.

WORKUP

后处理

  1. customequipped with a stirrer, a condenser
  2. customwhile removing
  3. customTo an obtained reaction mixture liquid, 0.6 g of 29% sodium hydroxide aqueous solution
  4. additionwas added
  5. custom103.5 g of 2-methyl phenol was recovered from an organic phase by concentration under reduced pressure
  6. additionTo a concentrated liquid, 161 g of toluene and 46 g of water were added
  7. customThereafter, an aqueous phase was separated
  8. customremoved
  9. customa target substance partitioned in an organic phase
  10. customwas recovered
  11. washThe organic phase was further washed twice with 46 g of water
  12. temperaturecooled to 10° C
  13. customThen, precipitated crystals
  14. filtrationwere subjected to filtration
  15. customdrying