Réaction #1162802

Équation de réaction

sodium perchlorate

5,5,8,8-tetramethyl-5,6,7,8tetrahydronaphthalen-2-ol

sodium hydroxide

sodium iodide

hydrochloric acid

sodium thiosulfate

→

3-iodo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-ol

Solvants

methanol

Conditions de réaction

Traitement

1. 1
   TempératureThe mixture was maintained
2. 2
   workup.STIRRINGAfter stirring
3. 3
   ExtractionIt was extracted with 200 ml of ethyl ether
4. 4
   LavageThe organic phase was washed twice with 400 ml of water
5. 5
   Séchagedried over magnesium sulfate
6. 6
   Concentrationconcentrated in a rotary evaporator under vacuum at 40° C.

Mode opératoire

A 3.6% sodium perchlorate solution was added dropwise to a mixture of 5,5,8,8-tetramethyl-5,6,7,8tetrahydronaphthalen-2-ol(6.35 g, 31.1 mmol), sodium hydroxide (1.23 g, 34.2 mmol) and sodium iodide (4.6 g, 31.1 mmol) in methanol (115 ml), at 0° C. The mixture was maintained under stirring for two hours at 0° C. 33 ml of a 10% sodium thiosulfate solution were added. After stirring, the mixture was acidified with hydrochloric acid to pH 1. It was extracted with 200 ml of ethyl ether. The organic phase was washed twice with 400 ml of water, dried over magnesium sulfate and concentrated in a rotary evaporator under vacuum at 40° C.

Source