Synthetic Route of 702-24-9, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 702-24-9, name is 4-Methoxy-N-methylbenzylamine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.
General procedure: A mixture of Ph3P (3148 mg, 12 mmol, 1 equiv) and hexachloroethane (2982 mg, 12.6 mmol, 1.05 equiv) in CHCl3 (total volume 40 mL) was stirred at 65 °C for 8 h. After cooling to r.t., under N2, to the mixture was added saccharin (7690 mg, 42.0 mmol, 3.5 equiv) in one portion, followed by the addition of the stock solution of DIPEA in CHCl3 (1.32 M, 59 mL, 78 mmol, 6.5 equiv). The resulting mixture was heated under N2 at 60 °C for 6 h. The mixture was cooled to r.t. and filtered under N2. The solid crude was washed with CHCl3 (3 × 5 mL) and dried under vacuum. The dry solid (5410 mg) was kept under N2. No further separation was attempted, and the resulting solid was used directly in the parallel chemistry. The total yield from Ph3P to the solid was assumed to be 100percent, thus the theoretical amount of the ?active? mixture of 13 and 14 was 451 mg/mol. Parallel Chemistry; General Procedure (Scheme 5) Under N2, to a mixture of the dry solid 13/14 (226 mg, 0.5 mmol) was added a stock solution of DIPEA (1.5 M, 2.17 mL, 3.25 mmol, 6.5 equiv) in CHCl3 at r.t. The mixture was stirred at r.t. for 5 min before a solution of the appropriate amine (1.0 mmol, 2 equiv) in CHCl3 (2 mL) was added. If the amine was in the form of HCl salt, 1 equiv extra of DIPEA was added to the reaction mixture. The resulting mixture was stirred at r.t. for 20 h, and then heated at 60 °C for 15 min. The solvents were evaporated, and the dry residue was dissolved in DMSO (4 mL). The DMSO solution was submitted to purification group for isolation.
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 4-Methoxy-N-methylbenzylamine, other downstream synthetic routes, hurry up and to see.
Reference:
Article; Chen, Yantao; Aurell, Carl-Johan; Korsgren, Pernilla; Malm, Johanna; Haerslaett, Malin; Friden-Saxin, Maria; Pettersen, Anna; Synthesis; vol. 50; 7; (2018); p. 1471 – 1481;,
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