1-(5-AMINO-2-METHYL-2-PHENYL-[1,3,4]THIADIAZOL-3-YL)-ETHANONE synthesis
- Product Name:1-(5-AMINO-2-METHYL-2-PHENYL-[1,3,4]THIADIAZOL-3-YL)-ETHANONE
- CAS Number:72926-06-8
- Molecular formula:C11H13N3OS
- Molecular Weight:235.31
2302-93-4
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108-24-7
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72926-06-8
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Yield:72926-06-8 76%
Reaction Conditions:
with pyridine at 20; for 12 h;
Steps:
11 Example 11 (Compound 14)
To acetophenone=thiosemicarbazone (10.0 g, 51.8 mmol) prepared in Step 1 of Example 1 was added acetic anhydride (4.90 mL, 51.9 mmol) and pyridine (8.40 mL, 104 mmol), and the mixture was stirred at room temperature for 12 hours. After the reaction mixture was concentrated under reduced pressure, ethyl acetate and 2 mol/L aqueous sodium hydroxide was added, and the mixture was subjected to separation. The organic layer was washed with saturated aqueous ammonium chloride and saturated aqueous sodium chloride, and dried over anhydrous sodium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/n-hexane = 1/1) to obtain Compound 14 (9.22 g, 76%).1H NMR (270 MHz, DMSO-d6) δ (ppm): 2.12 (s, 3H), 2.31 (s, 3H), 6.49 (br s, 2H), 7.21-7.41 (m, 5H)
References:
EP1454903,2004,A1 Location in patent:Page 40
72926-24-0
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$28.00/1mg
72926-06-8
16 suppliers
$378.00/1g