Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List 2,4-DIAMINO-6-HYDROXY-5-THIOCYANOPYRIMIDINE

2,4-DIAMINO-6-HYDROXY-5-THIOCYANOPYRIMIDINE synthesis

2synthesis methods
-

Yield:22288-75-1 100%

Reaction Conditions:

Stage #1: potassium thioacyanate;2,6-diaminopyrimidin-4-olwith acetic acid at 25 - 95;Inert atmosphere;
Stage #2: with bromine at 10 - 20; for 2 h;

Steps:

1.1 Step 1: 2,6-diamino-5-thiocyanatopyrimidin-4-ol:

To a stirred solution of Acetic acid (27500 mL) in a reactor at 25-30 °C under Nitrogen atmosphere was added 2, 6- diaminopyrimidin-4-ol (500 g). Potassium thiocyanate (1586 g) was added slowly and the temperature was raised to 90±5 °C; until the reaction mass becomes a clear solution. Once it becomes a clear solution, the reaction mixture was cooled to 15±5 °C and bromine (633 g) in acetic acid (750 mL) was added drop wise, stirred for 2 h at the same temperature. After the completion of the reaction, the reaction mixture was neutralised using aqueous ammonia (9000 mL) and stirred for 16 h at 20±5 °C. The precipitate formed was filtered and rinsed with water (2500 mL) and methanol (1000 mL). The wet material was dried in VTD at 70 °C for 24 hours to give the title compound as a pale yellow solid (206 g, quant). LCMS: 184.3 [M+l] +.1H-NMR (400 MHz, DMSO-d6): δ 10.36 (s, 1H), 7.03 (s, 2H), 6.64 (bs, 2H).

References:

WO2018/178338,2018,A1 Location in patent:Page/Page column 81-82