Continuously updated synthesis method about 627-31-6

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3-Diiodopropane(stabilized with Copper chip), and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 627-31-6, Application In Synthesis of 1,3-Diiodopropane(stabilized with Copper chip)

A THF solution (12 mL) of the above-mentioned colorless oily matter (153 mg, 0.45 mmol) was cooled to -40 C., and LDA (0.7 mL, 1.4 mmol) was then added. This was stirred at -40 C. for 0.5 hour. Thereafter 1,3-diiodopropane (0.26 mL, 2.3 mmol) was added thereto, which was then stirred at -40 C. for three hours. After that, a saturated ammonium chloride aqueous solution was added. Subsequently, the organic layer was separated and an aqueous layer was extracted with ethyl acetate. The mixed organic layer was washed with saturated saline, dried with anhydrous sodium sulfate, and concentrated under reduced pressure. The crude extract thus obtained was purified using column chromatography (n-hexane:ethyl acetate=4:1). Thus MI-22 (22 mg, 21%) was obtained as a colorless oily matter. The respective data of the infrared (IR) absorption spectrum, the nuclear magnetic resonance (1H, 13C-NMR) spectrum, and the mass spectrometry (FAB) of the MI-22 are indicated below: IR (KBr) 3416, 2855, 1614 cm-1; 1H NMR (CDCl3, 300 MHz): delta 0.88 (6H, t, J=6.4 Hz), 1.09 (6H, t, J=7.2 Hz), 1.14 (6H, t, J=7.2 Hz), 1.20-1.38 (48H, m), 1.50-1.62 (2H, m), 1.98-2.03 (8H, m), 2.42-2.52 (2H, m), 3.31 (4H, q, J=7.2 Hz), 3.36 (4H, q, J=7.2 Hz), 5.32-5.35 (4H, m); 13C NMR (CDCl3, 300 MHz): delta 12.9, 13.9, 14.8, 22.5 (2C), 27.0 (2C), 27.4, 29.0 (3C), 29.3, 29.6 (2C), 31.7 (2C), 33.3, 33.5, 40.2, 41.0, 41.6, 129.5, 129.7, 175.1; and LRMS (FAB) m/z 716 (MH+). HRMS (FAB) calcd for C47H91N2O2, 715.7081; found, 715.7078.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3-Diiodopropane(stabilized with Copper chip), and friends who are interested can also refer to it.

Reference:
Patent; Nojima, Hiroshi; Kita, Yasuyuki; US2008/89924; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com