Reaktion #1435739

Reaktionsgleichung

N-[4-iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-yl]-2,2-dimethyl-propionamide

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title compound

Ausbeute 92.0%

4-Iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-ylamine

Ausbeute 92.0%

Lösungsmittel

hydrochloric acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling to 0° C. the reaction mixture
2. 2
   Waschenwas washed twice with ether (50 ml)
3. 3
   workup.ADDITIONThe aqueous phase was treated with 50 ml dichloromethane
4. 4
   SonstigeThe organic phase was separated
5. 5
   Extraktionthe aqueous phase was extracted four times with 50 ml dichloromethane
6. 6
   TrocknenThe combined organic layers were dried over sodium sulfate
7. 7
   Einengenconcentrated in vacuo

Vorschrift

A mixture of 2.20 g (5.47 mmol) N-[4-iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-yl]-2,2-dimethyl-propionamide (synthesis described in DE10008042) in 50 ml 3 N hydrochloric acid was stirred for 18 h at 100° C. After cooling to 0° C. the reaction mixture was washed twice with ether (50 ml). The aqueous phase was treated with 50 ml dichloromethane and basified with a 1 M solution of sodium carbonate. The organic phase was separated and the aqueous phase was extracted four times with 50 ml dichloromethane. The combined organic layers were dried over sodium sulfate and concentrated in vacuo to give 1.60 g (92%) of the title compound as an off-white solid.

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