Reaktion #66186

Reaktionsgleichung

compound

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

azetidine

→

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

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigereacted at 120° C. in a single-mode microwave oven (CEM Explorer) for 40 min
2. 2
   FiltrationThe solid is filtered off
3. 3
   Waschenwashed twice with in each case 0.5 ml of ethanol
4. 4
   Sonstigethe solvent is removed on a rotary evaporator
5. 5
   SonstigeThe residue is purified by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient with addition of 0.1% TFA)
6. 6
   Einengenconcentrated on a rotary evaporator
7. 7
   Temperaturunder reflux in ethanol for 20 min
8. 8
   Filtrationfiltered off while still hot
9. 9
   SonstigeThe solid obtained
10. 10
    Sonstigeis dried under high vacuum

Vorschrift

150 mg (0.5 mmol) of the compound from Example 23 and 63 mg (1 l mmol) of azetidine are suspended in 4 ml of ethanol and reacted at 120° C. in a single-mode microwave oven (CEM Explorer) for 40 min. The solid is filtered off, washed twice with in each case 0.5 ml of ethanol and discarded. The mother liquor is combined with the wash solutions, and the solvent is removed on a rotary evaporator. The residue is purified by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient with addition of 0.1% TFA). The product-containing fractions are combined and concentrated on a rotary evaporator. The residue is stirred under reflux in ethanol for 20 min and then filtered off while still hot. The solid obtained is dried under high vacuum.

Quelle