반응 #66180

반응 방정식

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

용매

THF

반응 조건

후처리

1. 1
   기타The reaction mixture is reacted in a single-mode microwave oven (Emrys Optimizer) at 120° C. for 24 min
2. 2
   기타The cooled reaction solution
3. 3
   농축is then concentrated on a rotary evaporator
4. 4
   기타the 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
   농축The suspension is then concentrated under reduced pressure
7. 7
   기타the residue is dried

실험 절차

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.

출처