Reaktion #2200667

Reaktionsgleichung

water

(R)-1-(but-2-ynyl)-2-(3-tert-butoxycarbonylamino-piperidin-1-yl)-5-methyl-5,6-dihydro-1H-imidazo[4,5-d]pyridazine-4,7-dione

potassium carbonate

3-methyl-isoquinolin-1-ylmethyl-chloride

→

(R)-1-(but-2-ynyl)-2-(3-tert-butoxycarbonylamino-piperidin-1-yl)-5-methyl-6-(3-methyl-isoquinolin-1-ylmethyl)-5,6-dihydro-1H-imidazo[4,5-d]pyridazine-4,7-dione

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionis extracted three times with ethyl acetate
2. 2
   Trocknenthe combined organic phases are dried over sodium sulphate
3. 3
   Sonstigethe solvent is removed
4. 4
   SonstigeThe residue is purified over silica gel (cyclohexane/ethyl acetate 1:1)

Vorschrift

0.20 g of (R)-1-(but-2-ynyl)-2-(3-tert-butoxycarbonylamino-piperidin-1-yl)-5-methyl-5,6-dihydro-1H-imidazo[4,5-d]pyridazine-4,7-dione and 0.10 g potassium carbonate are placed in 2 ml of dimethylformamide. Then 0.10 g of 3-methyl-isoquinolin-1-ylmethyl-chloride are added and the mixture is stirred for 5 h at 50° C. After the addition of water the mixture is extracted three times with ethyl acetate, the combined organic phases are dried over sodium sulphate, and the solvent is removed. The residue is purified over silica gel (cyclohexane/ethyl acetate 1:1).

Quelle