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ChemicalBook CAS DataBase List GSK J4 HCl
1373423-53-0

GSK J4 HCl synthesis

3synthesis methods
-

Yield:-

Reaction Conditions:

in dimethyl sulfoxide;

Steps:

Ethyl N-[2-(2-pyridinyl)-6-(1,2,4,5-tetrahydro-3H-3-benzazepin-3-yl)-4-pyrimidinyl]-β-alaninate

Ethyl N-[2-(2-pyridinyl)-6-(1,2,4,5-tetrahydro-3H-3-benzazepin-3-yl)-4-pyrimidinyl]-β-alaninate
To a microwave vial with a stirrer was added 2,3,4,5-tetrahydro-1H-3-benzazepine (0.049 mL, 0.326 mmol), ethyl N-[6-chloro-2-(2-pyridinyl)-4-pyrimidinyl]-β-alaninate (100 mg, 0.326 mmol), DIPEA (0.114 mL, 0.652 mmol) and Dimethyl Sulfoxide (DMSO) (0.5 mL).
The reaction vessel was sealed and heated in a Biotage Initiator microwave to 150 °C for 2.5 hr.
After allowing the reaction mixture to cool, analysis by LCMS showed 73% conversion to the product.
The reaction mixture was dissolved in DMSO to make the sample up to 1 mL and purified by MDAP. Product containing fractions were combined and the solvent evaporated in vacuo to give the title compound (99 mg) as a yellow oil.

References:

EP2592154,2013,A1 Location in patent:Page/Page column

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