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. 1871-57-4, name is 3-Chloro-2-chloromethyl-1-propene, A new synthetic method of this compound is introduced below., Quality Control of 3-Chloro-2-chloromethyl-1-propene
Sodium hydride (60% in mineral oil) (0.99 g, 24.81 mmol) was dissolved in DMF (20 mL) at 0 C and 3-chloro-2-(chloromethyl)prop-1-ene (1.31 mL, 12.41 mmol) was added in portions. Separately N-boc-ethanolamine (1.92 mL, 12.41 mmol) was dissolved in THF (20 mL) and added dropwise. The reaction mixture was stirried at 20 C for 21 h. The volatiles were removed under reduced pressure. The reaction was diluted with water (50 mL) and then extracted with EtOAc (3 x 80 mL). The organic extracts were combined passed through a phase separation cartridge and the volatiles were removed under reduced pressure. The crude product was dissolved in DCM and purified via silica gel chromatography eluting with 0-50% EtOAc in heptane to afford tert-butyl 6-methylene-1,4-oxazepane-4-carboxylate (1.25 g, 47%) as a clear oil. 1H NMR (400 MHz, CDCl3) 1.46 (s, 9H), 3.37 – 3.45 (m, 2H), 3.64 – 3.79 (m, 2H), 4.00 – 4.24 (m, 4H), 4.88 – 5.04 (m, 2H); 13C NMR (400 MHz, DMSO, 100 C) 28.58, 50.40, 51.72, 71.82, 74.29, 79.44, 112.06, 146.96, 154.80; HRMS [M+H]+ measured 236.1274, C11H19NO3 requires 236.1263.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Article; Watson, David W.; Gill, Matthew; Kemmitt, Paul; Lamont, Scott G.; Popescu, Mihai V.; Simpson, Iain; Tetrahedron Letters; vol. 59; 51; (2018); p. 4479 – 4482;,
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