Reaktion #2173405

Reaktionsgleichung

1-(tert-butoxycarbonylamino)-2-piperazinone

sodium carbonate

6-chloronaphthalene-2-sulfonyl chloride

→

1-(tert-butoxycarbonylamino)-4-(6-chloronaphthalene-2-sulfonyl)-2-piperazinone

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe organic phase was separated
2. 2
   Waschenwashed with brine
3. 3
   Sonstigedried
4. 4
   Einengenconcentrated
5. 5
   SonstigeThe residue thus obtained
6. 6
   Sonstigewas purified by a column chromatography on a silica gel (hexane:ethyl acetate=1:2)

Vorschrift

The resultant solution of 1-(tert-butoxycarbonylamino)-2-piperazinone in ethyl acetate (20 ml) and a 10% aqueous solution of sodium carbonate (20 ml) was treated at 0° C. with 6-chloronaphthalene-2-sulfonyl chloride (1.36 g) and stirred at room temperature for 30 minutes. The organic phase was separated, washed with brine, dried and concentrated. The residue thus obtained was purified by a column chromatography on a silica gel (hexane:ethyl acetate=1:2) to obtain 1-(tert-butoxycarbonylamino)-4-(6-chloronaphthalene-2-sulfonyl)-2-piperazinone (848 mg) as a colorless amorphous solid.

Quelle