反応 #217456

反応方程式

hydrochloric acid

2-acetyl-7-(4-allyloxybutyloxy)fluorene

Sodium hypobromite

sodium hydroxide

bromine

sodium thiosulfate

→

2-(4-allyloxybutyloxy)fluorene-7-carboxylic acid

溶媒

dioxane

water

反応条件

後処理

1. 1
   workup.ADDITIONwas dropwise added
2. 2
   workup.ADDITIONafter finishing dropwise adding
3. 3
   温度The reaction mixture was cooled to 10° C.
4. 4
   ろ過was filtered
5. 5
   その他dried
6. 6
   その他The solid matter was recrystallized from acetic acid

実験手順

A dioxane (380 ml) solution of 2-acetyl-7-(4-allyloxybutyloxy)fluorene 22 g was cooled to 8° C. Sodium hypobromite prepared from water 209 ml, sodium hydroxide 42.7 g and bromine 15.2 ml was dropwise added thereto, and after finishing dropwise adding, the solution was stirred at 40° C. for 15 minutes. The reaction mixture was cooled to 10° C., and then a saturated sodium thiosulfate aqueous solution was added thereto. A solid matter deposited by acidifying the solution with hydrochloric acid was filtered and then dried. The solid matter was recrystallized from acetic acid to obtain 15 g of 2-(4-allyloxybutyloxy)fluorene-7-carboxylic acid. Phase transition temperature: C164N222I.

出典