4(1H)-Pyrimidinone, 6-methyl-2-[(phenylmethyl)thio]- synthesis
- Product Name:4(1H)-Pyrimidinone, 6-methyl-2-[(phenylmethyl)thio]-
- CAS Number:3019-17-8
- Molecular formula:C12H12N2OS
- Molecular Weight:232.3
Yield:3019-17-8 83 %
Reaction Conditions:
Stage #1: 6-methyl-2-thiouracilwith potassium carbonate in N,N-dimethyl-formamide at 20;
Stage #2: benzyl chloride in N,N-dimethyl-formamide;
Steps:
32.2-33.2
(2) At room temperature, add intermediate 1 (1.0 equivalent, 1.0 g, 7.03 mmol), K2CO3(1.5 equivalents, 0.77g, 10.55mmol) and 30ml DMF, stirred for 0.25h, slowly added iodomethane (1.2 equivalents, 1.20g, 8.44mmol) dropwise, stirred overnight (12h), TLC monitored the end of the reaction.It was quenched by adding 20 mL of water, extracted with ethyl acetate (20 mL×3), combined the organic phases, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to obtain a crude product.The crude product was recrystallized from ethanol to obtain 6-methylpyrimidine-2-methylsulfide (intermediate 2), yield: 80%.
References:
CN115385862,2022,A Location in patent:Paragraph 0039; 0042; 0194; 0197; 0199; 0202
