Electric Literature of 24599-58-4, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 24599-58-4 name is 2,5-Dimethoxytoluene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
2,5-dimethoxy toluene 1 (9.0 g, 59.21 mmol) in diethyl ether (90 cm3) was added to a stirred solution of iodine monochloride (10.17 g, 62.65 mmol) in chloroform (30 cm) over 30 minutes. The mixture was stirred overnight before 10% sodium thiosulfate (150 cm3) was added. The organics were extracted with 2×75 cm3) of diethyl ether. The organics were combined, washed with saturated aqueous NaHCO3 (150 cm3), brine (100 cm3), dried (MgSO4) and dried under vacuum. The resultant solid was recrystallised from methanol to yield the title compound as red solid 2 (11.3 g, 69%). [0085] Rf 0.52 (SiO2, Hex 3:1 EtOAc). [0086] Mp 80-82 C. (Literature 81-82 C. (Reed et al., JACS, 120(38): 9729-9734, 1998) [0087] 1H NMR (400 MHz, CDCl3) 2.12 (3H, s, CH), 3.72 (3H, s, OCH), 3.75 (3H, s, OCH), 6.60 (1H, s, ArH), 7.10 (1H, s, ArH) ppm.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,5-Dimethoxytoluene, and friends who are interested can also refer to it.
Reference:
Patent; Onco-NX Limited; Mcgown, Alan; Hadfield, John; Butler, John; US2015/210639; (2015); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem