The chemical industry reduces the impact on the environment during synthesis 821-99-8, name is 1,9-Dichlorononane, I believe this compound will play a more active role in future production and life. 821-99-8
General procedure: To a DMF solution (63 mL) of 3b (1.06 g, 6.31 mmol) was added sodium hydride (55% oil dispersion, 340 mg, 7.8 mmol) at rt. After being stirred for 2 h at rt, the suspension was cooled to 0 C, and 1,8-dichlorooctane (3.40 mL, 3.47 g, 18.9 mmol) was added to the suspension. The mixture was allowed to warm to rt and stirred at rt for 2 h and then at 55 C for 10 h. After adding aqueous HCl solution (35%, 0.7 mL) at rt, the mixture was concentrated under reduced pressure and diluted with water (30 mL). The aqueous solution was washed with hexane (320 mL), treated with NaHCO3 until the pH reached to 9, and extracted with AcOEt (3*150 mL). The organic layers combined were washed with water (3500 mL), dried over anhydrous Na2SO4, concentrated under reduced pressure, and subjected to silica gel column chromatography (CHCl3/MeOH 100:0 to 96:4, v/v) to afford 4b[11] as a colorless oil (1.25 g, 3.97 mmol, 63%). Because 4b[11] tends to undergo inter- and intramolecular quaternization during storage, the obtained material was characterized only by 1H NMR and used for the next reaction immediately after the purification. 1H NMR (300 MHz, CDCl3, 25 C, TMS): delta=0.73 (3H, d, 3JH-H=6.6 Hz), 1.05 (3H, d,3JH-H=6.9 Hz), 1.24-1.34 (5H, m), 1.36-1.44 (2H, m), 1.47-1.51 (2H, m), 1.67-1.81 (3H, m), 2.08-2.19 (1H, m), 2.37 (3H, s), 3.24-3.39 (2H, m), 3.53 (2H, t, 3JH-H=6.9 Hz), 3.63-3.75 (3H, m), 6.92-6.93 ppm (2H, m).
The chemical industry reduces the impact on the environment during synthesis 821-99-8. I believe this compound will play a more active role in future production and life.
Reference:
Article; Noguchi, Tomohisa; Li, Chunji; Sasaki, Daisuke; Yamada, Kuniyo; Saigo, Kazuhiko; Ishida, Yasuhiro; Tetrahedron; vol. 72; 11; (2016); p. 1493 – 1504;,
Chloride – Wikipedia,
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