Reaktion #666987

Reaktionsgleichung

2-(bromomethyl)-2,3-dihydro-1,4-benzodioxin

6-chloro-N-(4-piperidinylmethyl)-2-benzothiazolamine dihydrobromide

sodium carbonate

sodium iodide

→

6-chloro-N-[[1-[(2,3-dihydro-1,4-benzodioxin-2-yl)methyl]-4-piperidinyl]-methyl]-2-benzothiazolamine

Ausbeute 59.8%

Lösungsmittel

N,N-dimethylacetamide

Water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe product was extracted with 4-methyl-2-pentanone
2. 2
   SonstigeThe extract was dried
3. 3
   Filtrationfiltered
4. 4
   Sonstigeevaporated
5. 5
   SonstigeThe oily residue was crystallized from a mixture of 1,1'-oxybisethane and 2,2'-oxybispropane
6. 6
   FiltrationThe product was filtered off
7. 7
   Sonstigedried

Vorschrift

A mixture of 1.9 parts of 2-(bromomethyl)-2,3-dihydro-1,4-benzodioxin, 3.3 parts of 6-chloro-N-(4-piperidinylmethyl)-2-benzothiazolamine dihydrobromide, 5 parts of sodium carbonate, 0.1 parts of sodium iodide and 67.5 parts of N,N-dimethylacetamide was stirred overnight at about 75° C. Water was added to the reaction mixture and the product was extracted with 4-methyl-2-pentanone. The extract was dried, filtered and evaporated. The oily residue was crystallized from a mixture of 1,1'-oxybisethane and 2,2'-oxybispropane. The product was filtered off and dried, yielding 1.8 parts (59.8%) of 6-chloro-N-[[1-[(2,3-dihydro-1,4-benzodioxin-2-yl)methyl]-4-piperidinyl]-methyl]-2-benzothiazolamine; mp. 155.8° C. (compound 16).

Quelle