Reaktion #969900

Reaktionsgleichung

product

8-[4-(benzyloxy)phenoxy]-2,3,4,5-tetrahydro-1,2,5-benzothiadiazepine 1,1-dioxide

→

4-[(1,1-dioxido-2,3,4,5-tetrahydro-1,2,5-benzothiadiazepin-8-yl)oxy]-phenol

Lösungsmittel

ethanol

dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe catalyst is removed by filtration
2. 2
   Sonstigethe filtrate is evaporated to dryness
3. 3
   WaschenThe organic phase is washed with 1% NaHCO3 solution
4. 4
   Trocknenwith saturated NaCl solution, dried (MgSO4)
5. 5
   Filtrationfiltered
6. 6
   Sonstigeevaporated
7. 7
   SonstigeThe residue is triturated in a mixture of ethyl acetate/ethyl ether
8. 8
   Sonstigeto yield
9. 9
   Filtrationafter filtration

Vorschrift

The product of Example 8 (0.76 mmol) is hydrogenated for 1 hour at atmospheric pressure in 60 ml of ethanol in the presence of 30 mg of 10% palladium-on-carbon and 2 drops of 4N HCl solution in dioxane. The catalyst is removed by filtration and the filtrate is evaporated to dryness. The residue is taken up in the hot state in ethyl acetate. The organic phase is washed with 1% NaHCO3 solution and then with saturated NaCl solution, dried (MgSO4), filtered and evaporated. The residue is triturated in a mixture of ethyl acetate/ethyl ether to yield, after filtration, the title product.

Quelle