5-Pyrimidinol, 4-amino- (7CI,9CI) synthesis

Yield:52601-89-5 90%

Reaction Conditions:

with sodium methylate;1-dodecylthiol in N,N-dimethyl-formamide at 120; for 12 h;Inert atmosphere;

Steps:

53.1 first step4-amino-5-hydroxypyrimidine

4-Amino-5-methoxypyrimidine 53a (500.0 mg, 4.0 mmol) and sodium methoxide (432.0 mg, 8.0 mmol) were dissolved in anhydrous N,N-dimethylformamide (6.0 mL).To which was added dodecyl mercaptan (1.61 g, 8.00 mmol),Stir at 120 ° C for 12 hours. The reaction solution was cooled to room temperature and dehydrated under reduced pressure to give a crude material.The pH was adjusted to 5-6 with water (5.0 mL) and acetic acid (0.5 mL). The aqueous phase was washed with ethyl acetate (10 mL×5).Decompression under reduced pressure gave 4-amino-5-hydroxypyrimidine 53b (400.0 mg, 3.60 mmol,Off-white solid), yield 90%.

References:

CN109020957,2018,A Location in patent:Paragraph 0227