486460-21-3, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 486460-21-3, name is 3-(Trifluoromethyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo[4,3-a]pyrazine, A new synthetic method of this compound is introduced below.
The dihydroformed product prepared in Example 7 (1.5 g, 3.1 mmol) was added to 60 mL of 2N HCl,Reflux for 12 hours.Ice water bath cooling,The bottom of the yellow oil precipitation,Pour the upper water,The lower oily substance was dissolved in dichloromethane,A small amount of saturated sodium bicarbonate washing,Dispensing,After the organic phase is dried,With a rotary evaporator evaporated to dry yellow liquid,Directly take the next step.Ice water bath,A small amount of the above crude product (0.6 g, 1.4 mmol) was dissolved in dichloromethane (10 mL)Plus DIPEA (Chinese name: N, N-diisopropylethylamine, 452 mg, 3.5 mmol)And 1-hydroxybenzotriazole (19 mg, 0.14 mmol)Trimethylacetyl chloride (210 mg, 1.75 mmol) was then added dropwise.After 0.5 hours,A solution of 3- (trifluoromethyl) -5,6,7,8-tetrahydro- [1,2,4] triazolo [4,3-a] pyrazine (CAS No. 486460-21-3, 296 mg, 1.54 mmol),Continue stirring at room temperature overnight.The next day,Washed,Saturated sodium bicarbonate wash,Organic phase dry,With a rotary evaporator to dry the crude product,1.14 g (yield: 67%, HPLC purity 99%) was obtained by recrystallization (petroleum ether / ethyl acetate = 20/1) as a white solid amidated product.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Zhejiang Xinhecheng Co., Ltd.; Zhejiang University; Zhang Yuhong; Yao Jinzhong; Qian Hongsheng; Lin Cong; Lu Guobin; Tang Jiaxing; Shen Chuang; (15 pag.)CN103819475; (2017); B;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem