HRID78962

反应详情

EQUATION

反应方程式

HRID 78962 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A reaction was carried out in the same manner as in Example 3. To an obtained reaction mixture liquid, 135 g of toluene, 23 g of water, and 17.9 g of 29% sodium hydroxide aqueous solution were added, and the reaction mixture liquid was neutralized by stirring at 80° C. Thereafter, an aqueous phase was separated and removed. An organic phase was further washed twice with 23 g of water. From the organic phase, toluene and 91.5 g of 2-methyl phenol were distilled away by concentration under reduced pressure. Thereafter, 161 g of toluene was added to a concentrated liquid, and the mixture liquid was cooled to 10° C. Then, precipitated crystals were subjected to filtration and drying to obtain 37.0 g of 9,9-bis(4-hydroxy-3-methylphenyl)fluorene (yield: 82.5%, LC purity: 98.7%). 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 4 in Gardner. The total amount of toluene used in the production was 8 parts by weight relative to 1 part by weight of the 9,9-bis(4-hydroxy-3-methylphenyl)fluorene.

WORKUP

后处理

  1. additionwere added
  2. customThereafter, an aqueous phase was separated
  3. customremoved
  4. washAn organic phase was further washed twice with 23 g of water
  5. distillationFrom the organic phase, toluene and 91.5 g of 2-methyl phenol were distilled away by concentration under reduced pressure
  6. additionThereafter, 161 g of toluene was added to a concentrated liquid
  7. temperaturethe mixture liquid was cooled to 10° C
  8. customThen, precipitated crystals
  9. filtrationwere subjected to filtration
  10. customdrying