Reaktion #346507

Reaktionsgleichung

sodium hydroxide

4,5,6,7-tetrahydrobenzo[b]-thiophen-4-amine hydrochloride

chloroform

sulfuryl chloride

→

2-chloro-4,5,6,7-tetrahydrobenzo[b]thiophen-4-amine

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeat about 10° C.
2. 2
   workup.DISSOLUTIONto dissolve the suspended solid
3. 3
   Extraktionextracted with chloroform twice
4. 4
   SonstigeThe extracts are dried
5. 5
   Sonstigeevaporated to dryness
6. 6
   workup.DISTILLATIONthe residue is distilled

Vorschrift

A sample of 11.4 grams 4,5,6,7-tetrahydrobenzo[b]-thiophen-4-amine hydrochloride is stirred in 150 ml. of chloroform at about 10° C., and 6.1 ml. of sulfuryl chloride is added dropwise. The mixture is stirred for 3.5 hours at room temperature, and then about 20 ml. of 50% sodium hydroxide solution is added gradually to dissolve the suspended solid. The mixture is then poured into water and extracted with chloroform twice. The extracts are dried, evaporated to dryness, and the residue is distilled to give 7.4 grams of 2-chloro-4,5,6,7-tetrahydrobenzo[b]thiophen-4-amine, boiling point 94° C. to 98° C./0.5 Torr.

Quelle