Electric Literature of 3344-70-5,Some common heterocyclic compound, 3344-70-5, name is 1,12-Dibromododecane, molecular formula is C12H24Br2, 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.
In a two-necked flask under argon, NaH (43.7 mmol) is put into suspension in anhydrous THF (100 ml). The reaction medium is cooled down in an ice bath and acetoethyl acetate is added dropwise (39.7 mmol). After stirring for 10 minutes at 0° C. n-BuLi is added dropwise (1.56 M; 43.7 mmol). Stirring is carried out for a further 10 minutes at ambient temperature before proceeding with alkylation.Dibromododecane (15.9 mmol) in solution in 20 ml of anhydrous THF is added dropwise to the previous solution. The reaction medium is allowed to return to ambient temperature and stirring is continued for 1 hour. Water is added followed by extraction with ether (3 times). The organic phase is washed with a saturated NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness. The product is purified by chromatography on silica-gel eluting with AcOEt-Hexane (1-1). A white solid is obtained (Yield=65percent); M.p.=60° C.NMR 1H (200 MHz, CDCl3): d 4.16 (q, 4H, 2CH2), 3.41 (s, 4H, 2CH2), 2.50 (t, 4H, 2CH2), 1.56-121 (m, 30H).
The synthetic route of 3344-70-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; CNRS; US6972343; (2005); B1;,
Bromide – Wikipedia,
bromide – Wiktionary