4-Amino-2,4-dihydro-5-(1-methylethyl)-3H-1,2,4-triazol-3-one synthesis
- Product Name:4-Amino-2,4-dihydro-5-(1-methylethyl)-3H-1,2,4-triazol-3-one
- CAS Number:96240-10-7
- Molecular formula:C5H10N4O
- Molecular Weight:142.16
Yield: 73.1%
Reaction Conditions:
Stage #1:carbonodihydrazide with lithium hydroxide in tolueneReflux;
Stage #2:Methyl isobutyrate in toluene at 105 - 110; for 4 h;
Steps:
2
Put 100 mL of toluene into a 500 mL four-necked flask, start stirring, put 86.4 g (0.95 mol) carbohydrazide and 26.4 g (1.09 mol) lithium hydroxide, and heat to reflux. 102.1g (0.99mol) methyl isobutyrate was added dropwise at reflux temperature, and the addition was completed in about 2 hours. Incubate at 105-110°C for 2 hours. After the reaction is complete, the toluene is removed under negative pressure, and then 100 mL of water is poured in, cooled to 0°C for crystallization, filtered, and dried to obtain 100.7 g of white solid, which is the target product, with a purity of 98.0% and a yield of 73.1%.
References:
Beijing Yili Biological Technology Co., Ltd.;Wang Rui;Wang Wenjun;Gao Rui;Li Mengfei;Liu Wei;Wu Shaoxiang CN111808035, 2020, A Location in patent:Paragraph 0034; 0038-0040
