Reference of 4333-56-6, These common heterocyclic compound, 4333-56-6, name is Bromocyclopropane, its 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.
To a stirred suspension of magnesium turnings (300 mg, 12.3 mmol) in THF (2.0 mL) was added commercially available cyclopropyl bromide (0.800 mL, 9.99 mmol) in THF (17.2 mL) dropwise at room temperature over 30 min. During this operation, the reaction continued refluxing without heating. After the addition of the halide was completed, the mixture was stirred at room temperature for 5 h. The concentration of this solution of 40 was determined by titration as shown below. Titration. After an exactly 0.150-mL aliquot of the Grignard solution of 40 was quenched with an exactly known volume (0.250 mL) of a 1.000 M HCl standard solution (purchased from Yoneyama Yakuhin Kogyo, Co., Ltd. (Japan)), the mixture was then titrated with a 0.500 M NaOH standard solution (purchased from Yoneyama Yakuhin Kogyo, Co., Ltd. (Japan)) (0.352 mL) with methyl orange as an indicator to determine its concentration to be 0.49 M. Thus, the yield of the Grignard reagent was 98% based on the halide. In several runs, the Grignard concentrations usually fell within a range between 0.48 and 0.51 M.
Statistics shows that Bromocyclopropane is playing an increasingly important role. we look forward to future research findings about 4333-56-6.
Reference:
Article; Sugano, Goshi; Kawada, Kojiro; Shigeta, Masayuki; Hata, Takeshi; Urabe, Hirokazu; Tetrahedron Letters; vol. 60; 13; (2019); p. 885 – 890;,
Bromide – Wikipedia,
bromide – Wiktionary