Reaktion #619093

Reaktionsgleichung

water

4-Methyl-5-(4-methyl-piperazine-1-sulfonyl)-thiazol-2-ylamine

CDI

dicyclohexylamine

→

title compound

Ausbeute 4.0%

1,1-Dicyclohexyl-3-[4-methyl-5-(4-methyl-piperazine-1-sulfonvl)-thiazol-2-yl]-urea

Ausbeute 4.0%

Lösungsmittel

DCM

dichloroethane

dichloroethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigePrepared in the microwave oven (EmrysOptimizer®)
2. 2
   workup.ADDITIONwas added through the septum
3. 3
   Temperaturthe reaction mixture was heated for additional 600 sec
4. 4
   Sonstigeat 120° C
5. 5
   ExtraktionThe water phase was extracted with DCM (3×25 ml)
6. 6
   Trocknendried with MgSO4
7. 7
   Filtrationfiltered
8. 8
   Sonstigeevaporated in vacuo

Vorschrift

Prepared in the microwave oven (EmrysOptimizer®). 4-Methyl-5-(4-methyl-piperazine-1-sulfonyl)-thiazol-2-ylamine (0.04 g; 0.141 mmol), CDI (0.023 g; 0.141 mmol) and DMAP were mixed dichloroethane (1.5 ml) in a microwave vessel (2.5 ml). The reaction mixture was healed 600 sec at 120° C., dicyclohexylamine (0.025 g; 0.141 mmol) dissolved in dichloroethane (0.2 ml) was added through the septum and the reaction mixture was heated for additional 600 sec. at 120° C. To the reaction mixture was added water and DCM (25 ml). The water phase was extracted with DCM (3×25 ml), dried with MgSO4 filtered and evaporated in vacuo to afford the title compound. (84 mg) as a yellow oil. Purification by prep. HPLC gave 3 mg (Yield: 4%)

Quelle