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33097-12-0

4,6-Dichloro-2-(methylthio)pyrimidine-5-carbaldehyde oxime synthesis

2synthesis methods
-

Yield:33097-12-0 80%

Reaction Conditions:

with hydroxylamine hydrochloride;acetic acid in ethanol at 20 - 60; for 2 h;

Steps:

57.57a

To the mixture of hydroxylamine hydrochloride (139 mg, 2.0 mmol), HOAc (0.113 mL, 2.0 mmol) and EtOH (5 mL) was added 4,6-dichloro-2-(methylthio)-5- pyrimidinecarbaldehyde (223 mg, 1.0 mol) to room temperature. The solution was then heated at 50 0C for about 1 hour, 60 0C for about 30 minutes and 70 0C for about 30 minutes before it was concentrated under vacuum and washed with H2O (10-20 mL) to afford 4,6-dichloro-2-(memylthio)-5-pyrimidinecarbaldehyde.oxime (190 mg, 80%). LC-MS m/z 238 (M + H)+ 1.57 minute, 1.65 minute; 1H-NMR (CDCl3) δ 2.62, 2.65 (3 H), 7.53, 8.30 (1 H).

References:

WO2006/104917,2006,A2 Location in patent:Page/Page column 81-82