Electric Literature of 3250-73-5, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 3250-73-5 as follows.
EXAMPLE 9 To a solution of (ether)benzoxy alcohol 20A (501.2 mg, 2.751 mmol) in CH2Cl2 (20 mL) was added Et3N (509 mg, 5.03 mmol) and toluenesulfonyl chloride (623 mg, 3.27 mmol) at 5-10 C. After being stirred at 25 C. for 30 min, the reaction mixture was quenched with saturated aqueous Na2CO3 (20 mL) and extracted with ethyl acetate (3*50 mL). The combined organic layers were dried over MgSO4 (s), filtered, and concentrated under reduced pressure to obtain (ether)benzoxy tosylate 21A (853.5 mg, 2.539 mmol) as white solids in 92% yield: mp (recrystallized from CH2Cl2 and CCl4) 82-83 C.; 1H NMR (CDCl3, 300 MHz) delta 1.43 (t, J=10.2 Hz, 3 H, OCH2CH3), 2.51 (s, 3 H, ArCH3), 4.04 (q, J=10.2 Hz, 2 H, OCH2CH3), 4.36 (t, J=6.9 Hz, 2 H, OCH2CH2), 4.59 (t, J=6.9 Hz, 2 H, OCH2CH2), 6.86-6.97 (m, 4 H, ArH), 7.10-7.22 (m, 4 H, ArH); IR (neat) 3446 (br), 2982 (m), 2934 (m), 2884 (m), 1591 (s), 1558 (w), 1509 (s), 1478 (s), 1454 (s), 1407 (s), 1394 (s), 1371 (s), 1354 (s), 1279 (m), 1259 (s), 1247 (s), 1217 (s), 1178 (s), 1127 (s), 1066 (s), 1043 (s), 1031 (s), 977 (s), 929 (s), 905 (s), 809 (s), 776 (m), 749 (s), 776 (m) cm-1
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,3250-73-5, its application will become more common.
Reference:
Patent; Jih, Ru Hwu; Tsay, Shwu Chen; Magendran, Balaachary; Chakraborty, Subhasish K.; Das, Asish R.; Sheu, Kuen Wang; Shu, Chun Mei; Lu, Chin Kun; Chang, Wei Min; US2007/15939; (2007); A1;,
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