Reaktion #217456

Reaktionsgleichung

hydrochloric acid

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

Sodium hypobromite

sodium hydroxide

bromine

sodium thiosulfate

→

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

Lösungsmittel

dioxane

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas dropwise added
2. 2
   workup.ADDITIONafter finishing dropwise adding
3. 3
   TemperaturThe reaction mixture was cooled to 10° C.
4. 4
   Filtrationwas filtered
5. 5
   Sonstigedried
6. 6
   SonstigeThe solid matter was recrystallized from acetic acid

Vorschrift

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.

Quelle