In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 588-96-5 as follows. Recommanded Product: p-Bromophenetole
Step 1:Magnesium (8.24 g, 0.339 mol) was added to 300 mL of tetrahydrofuran (THF) in a reactor substituted with nitrogen atmosphere and dissolved by stirring. While keeping the internal temperature at 20 to 30 C, 4-bromophenetol 62 g, 0.308 mol) and 220 mL of tetrahydrofuran was slowly added thereto. After completion of the addition, the internal temperature was raised to 40 to 45 C and stirred for 2 hours. Step 2: In a reactor substituted with nitrogen atmosphere, (S)-tert-butyl 2-((R)-2,2-dimethyl-1,3-dioxolan-4-yl)aziridine-1-carboxylate (50 g, 0.206 mol) was added to 50 mL of toluene and dissolved with stirring, and CuBrS(CH3)2 (0.4 g, 0.002 mol) was added thereto. The internal temperature was further stirred for 30 minutes while maintaining the internal temperature at 20 to 25 C,and the internal temperature was cooled to -40 C.The solution of 4-bromophenetol magnesium bromide prepared according to the above step 1 was slowly added while keeping the internal temperature at -40 C or lower.After completion of the addition, the internal temperature was raised to -30 to -20 C and stirred for 1 hour. When the reaction was complete, 400 mL of 10% acetic acid aqueous solution and 400 mL of toluene were added to quench and separate.The separated oil layer was washed with 400 mL of a 7% sodium Sodium bicarbonate aqueous solution and 400 mL of purified water, and Sodium sulfate was added to dehydrate and then filtered.Thereafter, the filtrate was concentrated, 150 mL of methanol was added to the concentrated residue, stirred at an internal temperature of 20 to 25 C for 1 hour, and then filtered. The filtrate was concentrated again to give 75.1 g of the title compound tert-butyl (1S)-1-(2,2-dimethyl-1,3-dioxolan-4-yl)-2-(4-ethoxyphenyl)ethylcarbamate yield: 100 %
According to the analysis of related databases, 588-96-5, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Eseuti Pam Co., Ltd.; Kim Yeong-hun; Oh Jun-hyeon; Kang Sang-gyu; Jang Sun-gi; Im Geun-jo; (14 pag.)KR2018/50091; (2018); A;,
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