Reaktion #66180

Reaktionsgleichung

compound

2-(6-Chloropyrimidin-4-yl)-4-pyridin-3-yl-1,2-dihydro-3H-pyrazol-3-one

4-pyrrolidin-1-ylpiperidine

→

4-Pyridin-3-yl-2-[6-(4-pyrrolidin-1-ylpiperidin-1-yl)pyrimidin-4-yl]-1,2-dihydro-3H-pyrazol-3-one dihydrochloride

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe reaction mixture is reacted in a single-mode microwave oven (Emrys Optimizer) at 120° C. for 24 min
2. 2
   SonstigeThe cooled reaction solution
3. 3
   Einengenis then concentrated on a rotary evaporator
4. 4
   Sonstigethe residue is chromatographed by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient with addition of 0.1% formic acid)
5. 5
   workup.ADDITION1 ml of a 4 N solution of hydrogen chloride in dioxane is added to the resulting formate salt of the target compound
6. 6
   EinengenThe suspension is then concentrated under reduced pressure
7. 7
   Sonstigethe residue is dried

Vorschrift

100 mg (0.4 mmol) of the compound from Example 23 and 113 mg (0.7 mmol) of 4-pyrrolidin-1-ylpiperidine are initially charged in 3 ml of THF. The reaction mixture is reacted in a single-mode microwave oven (Emrys Optimizer) at 120° C. for 24 min. The cooled reaction solution is then concentrated on a rotary evaporator, and the residue is chromatographed by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient with addition of 0.1% formic acid). 1 ml of a 4 N solution of hydrogen chloride in dioxane is added to the resulting formate salt of the target compound, and the mixture is stirred at RT for 30 min. The suspension is then concentrated under reduced pressure, and the residue is dried.

Quelle