Application of 13831-03-3,Some common heterocyclic compound, 13831-03-3, name is tert-Butyl propiolate, molecular formula is C7H10O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Hexamethylphosphoric triamide (10.7 g, 59.9 mmol) was dissolved in tetrahydrofuran (160 mL) under nitrogen(0.5 M, 36 mL) was added at 0 C for 0.5 hour at 0 C, tert-butyl propiolate (5.04 g, 40 mmol) was added and the reaction was continued for 1 hour. Then add 2b (5.47g, 40mmol), gradually rose to room temperature, reaction 5 hours, slowly adding 1M hydrochloric acid to the reaction solution, adjust the reaction solution pH to 2 ~ 3, The organic phase was washed with saturated brine (100 mL x 1), dried over anhydrous sodium sulfate, filtered and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography and purified. The organic phase was extracted with ethyl acetate (50 mL x 2) (Ethyl acetate: petroleum ether (v / v) = 0: 1 to 1: 9) to give the title compound 2c as a yellow oil (2.2 g, yield 21%).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route tert-Butyl propiolate, its application will become more common.
Reference:
Patent; Sichuan Hai Sike Pharmaceutical Co., Ltd.; Wei Yonggang; Qiu Guanpeng; Lei Bolin; Li Yao; Wang Song; Zhu Guozhi; (39 pag.)CN106279128; (2017); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics