Application of 504-63-2, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 504-63-2, name is 1,3-Propanediol. A new synthetic method of this compound is introduced below.
Synthesis of Intermediate L Compound L was prepared according to the procedure of McDougal, P. G.; Rico, J. G.; Oh, Y.-L; Condon, B. J. Org. Chem., 1986, 51, 3388-3390. To a dried 250 mL RBF under an atmosphere of argon at room temperature was added 100 mL of distilled THF and 2.1 g of sodium hydride (60% dispersion in mineral oil; Aldrich). The mixture was stirred vigorously and 1,3-propanediol (4.0 g, 50 mmol; Aldrich) was added over 10 minutes via syringe. The reaction was allowed to stir for 45 minutes before tert-butyldimethylsilyl chloride (7.9 g, 52.7 mmol; Aldrich) was added portion wise over 5 minutes. The reaction was then allowed to stir for a further 45 minutes at room temperature before being quenched slowly with 20 mL of 10% aqueous sodium carbonate solution. This mixture was then transferred to a separatory funnel. After being vigorously shaken, the biphasic mixture was separated and the aqueous phase was further extracted with two 50 mL portions of ether. The combined organic phases are then dried with sodium sulfate and filtered through a plug of 1 inch of Celite and 1 inch of flash silica (silica gel 60, EMD) via a 100 mL sinter funnel under vacuum into a 500 mL RBF, with the sodium sulfate residue washed with a further 50 mL of ether. The collected solution was then reduced under vacuum on a Buchi rotary evaporator to give compound L, as a light yellow oil in 99% yield and >95% purity. The 1H NMR spectrum in CDCI3 agreed with the previously reported data. (See, McDougal, P. G.; Rico, J. G.; Oh, Y.-L; Condon, B. J. Org. Chem., 1986, 51, 3388-3390.)
At the same time, in my other blogs, there are other synthetic methods of this type of compound,504-63-2, 1,3-Propanediol, and friends who are interested can also refer to it.
Reference:
Patent; PREVACUS, INC.; THE FLORIDA STATE UNIVERSITY RESEARCH FOUNDATION, INC.; LEVY, Daniel, E.; CRAN, John, W.; (93 pag.)WO2016/44558; (2016); A1;,
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