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. 3722-78-9, name is 8-Bromochroman, A new synthetic method of this compound is introduced below., Recommanded Product: 3722-78-9
[0037] Prepare AP Ex 4 as follows. Add 8-bromochroman (407 mg, 1.91 mmol) in dry tetrahydrofuran (THF, 10 mL) cooled in a dry ice/acetone bath to a glass jar with a PTFE- coated stirbar. Stir the contents of the glass jar and add n-BuLi (2.5M in hexanes, 0.76 mL, 1.9 mmol) dropwise. Stir the contents of the glass jar at -78 C for 1.5 hrs. Add a suspension of chlorobis(2-methoxyphenyl)phosphine (482 mg, 1.72 mmol) in dry THF (15 mL) over the course of 10 minutes (min). Allow the contents of the glass jar to warm to 23 C. Stir the contents of the glass jar for 2 hrs at 23 C and remove volatiles with a rotary evaporator. Quench the reaction with water (10 mL) and wash with dichloromethane (DCM). Dry the organic layer over MgS04, filter, and remove volatiles with a rotary evaporator. Add the organic layer, warm ethanol (55 mL, 50 C), and DCM (8 mL) to a second glass jar to recrystallize the organic layer. Collect 2 crops of crystals from mother layer to yield AP Ex 4 (359 mg, 55% yield) in crystalline form. [0038] Analyze AP Ex 4 by XH, 13C, and 31P NMR spectroscopy to confirm formation. XH NMR (400 MHz, CDC13) delta 7.32 (t, J= 7.7 Hz, 2H), 7.03 (d, J= 7.5 Hz, 1H), 6.94 – 6.77 (m, 4H), 6.71 (t, J= 5.6 Hz, 3H), 6.53 – 6.42 (m, 1H), 4.10 (apparent t, J= 5.0 Hz, 2H), 3.75 (s, 6H), 2.81 (t, J= 6.4 Hz, 2H), 1.95 (dt, J= 11.4, 5.7 Hz, 2H); 13C NMR (101 MHz, CDC13) 6 161.61 (d, J= 16.8 Hz), 133.84 (s), 131.54 (s), 130.38 (s), 129.80 (s), 124.93 (d, J= 13.5 Hz), 123.63 (d, J= 12.8 Hz), 120.81 (s), 119.98 (s), 110.18 (s), 66.59 (s), 55.76 (s), 25.07 (d, J= 1.7 Hz), 22.31 (s); 31P NMR (162 MHz, CDC13) delta -38.86 (s).
The synthetic route of 3722-78-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; DOW GLOBAL TECHNOLOGIES LLC; CLARK, Thomas P.; SPINNEY, Heather A.; HOUSE, Sarah E.; BRIGGS, John R.; CUMMINS, Clark H.; KLINKENBERG, Jessica L.; WO2014/205025; (2014); A1;,
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