Reaktion #440010

Reaktionsgleichung

sodium chloride

1-(tert-butoxycarbonyl)-3,3-dimethylpiperazine

triethylamine

6-chloronaphthalene-2-sulfonyl chloride

→

4-(tert-Butoxycarbonyl)-1-[(6-chloronaphthalen-2-yl)sulfonyl]-2,2-dimethylpiperazine

Lösungsmittel

methylene chloride

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto form two layers
2. 2
   SonstigeThe organic layer obtained by separation
3. 3
   Trocknenwas dried over anhydrous sodium sulfate
4. 4
   Einengenconcentrated under reduced pressure
5. 5
   SonstigeThe crudely purified product was purified by chromatography on a silica gel column (hexane:ethyl acetate=8:1), whereby the title compound (155 mg)
6. 6
   Sonstigewas obtained as a colorless solid

Vorschrift

To a solution of 1-(tert-butoxycarbonyl)-3,3-dimethylpiperazine (125 mg) in methylene chloride (3.0 ml) were added triethylamine (90 ml) and 6-chloronaphthalene-2-sulfonyl chloride (167 mg). The resulting mixture was stirred at room temperature for 84 hours. The reaction mixture was diluted with methylene chloride and added with a saturated aqueous solution of sodium chloride to form two layers. The organic layer obtained by separation was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The crudely purified product was purified by chromatography on a silica gel column (hexane:ethyl acetate=8:1), whereby the title compound (155 mg) was obtained as a colorless solid.

Quelle