92001-52-0

Step 1: N-(4-amino-6-oxo-1,6-dihydropyrimidin-5-yl)acetamide (330 mg, 1.92 mmol, 1.00 eq., 98%) was dissolved in phosphorus oxychloride (5 mL) and the reaction was carried out at reflux overnight. After completion of the reaction, the mixture was concentrated under vacuum. The residue was redissolved in ethyl acetate (10 mL) and washed sequentially with saturated aqueous sodium bicarbonate (10 mL), water (10 mL) and brine (10 mL). The organic layer was dried over anhydrous sodium sulfate and concentrated in vacuum to give 6-chloro-8-methyl-9H-purine (20 mg, 6% yield) as a yellow solid.

[1] Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1984, # 5, p. 879 - 885
[2] Patent: US2012/202785, 2012, A1. Location in patent: Page/Page column 262