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36033-66-6

5-(methylsulfonyl)-1,3,4-thiadiazol-2-amine(SALTDATA: FREE) synthesis

2synthesis methods
-

Yield:98143-01-2 42%

Reaction Conditions:

at 60; for 1 h;

Steps:

N-(5-(Methylsulfonyl)-l,3,4-thiadiazol-2-yl)acetamide (30, AB2-V-007).

General procedure: In a vial was added 5-(methylsulfonyl)-l,3,4-thiadiazol-2-amine (0.050 g, 1 eq., 0.28 mmol) followed by acetic anhydride (0.043 g, 1.5 eq., 0.42 mmol) in acetic acid (1 ml). The reaction mixture was stirred at 60 °C for 1 h. The solution was gradually cooled followed by the addition of water (10 ml). The suspension was cooled to 0 °C and the target compound was collected by filtration as a white solid (0.026 g, 0.12 mmol, 42%). ' H NMR (500 MHz, DMSO-ifc): d 13.26 (s, 1H, NH), 3.52 (s, 3H, CH3), 2.27 (s, 3H, CH3). 13C NMR (126 MHz, DMSO -d6) d 170.0, 162.7, 162.6, 43.6, 22.7. HPLC retention time: 11.118 min. HPLC Purity: 100%.

References:

WO2020/131980,2020,A1 Location in patent:Paragraph 0082-0083; 00114

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