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ChemicalBook CAS DataBase List (2-Chloro-5-Methoxy-pyriMidin-4-yl)-Methyl-aMine
1351762-06-5

(2-Chloro-5-Methoxy-pyriMidin-4-yl)-Methyl-aMine synthesis

1synthesis methods
-

Yield:1351762-06-5 95%

Reaction Conditions:

in methanol;ethanol at 0; for 0.5 h;

Steps:

28.1 Step-1: 2-Chloro-5-methoxy-N-methylpyrimidin-4-amine

Step-1: 2-Chloro-5-methoxy-N-methylpyrimidin-4-amine [0168] At 0 °C, to a solution of 2,4-dichloro-5-methoxypyrimidine (5.2 g, 29.0 mmol) in MeOH (50 mL), a solution of methylamine in EtOH (8 M, 8.3 mL, 66.8 mmol) was added slowly, and then allowed the mixture to warm to room temperature for 30 min. TLC showed completed reaction. The reaction mixture was concentrated to dryness, and the solid was dissolved in dichloromethane and washed with saturated sodium bicarbonate. The organic layer was dried over magnesium sulfate and concentrated to give the desired product as white solid (4.80 g, 95%).1H NMR (300 MHz, CDCl3): δ 7.48 (s, 1H), 5.46 (bs, 1H), 3.85 (s, 3H), 3.04 (d, J = 4.9 Hz, 3H).

References:

WO2016/171755,2016,A1 Location in patent:Paragraph 0168