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. 69411-05-8, name is 3-Chloro-5-trifluoromethylaniline, A new synthetic method of this compound is introduced below., Recommanded Product: 69411-05-8
11568] 3-Chloro-5-trifluoromethylaniline (3.66 g, 18.7 mmol) was dissolved in 70 mE THF and stirred in an ice bath. To it were added 13oC2O (4.48 g, 20.6 mmol) and DMAP (2.51 g, 20.6 mmol). The mixture was stirred for overnight, and was concentrated in vacuo. The residue was taken into 200 mE EtOAc, washed with water x3, dried, rotavaped, and subjected to silica flash column using 1% MeOH in DCM to get tert-butyl 3-chloro-5-(trifluoromethyl)phenylcarbamate (466,3.37 g, 61%) as awhite solid. It was dissolved in 100 mE dry THF and treated with NaH (60% in mineral oil, 910 mg, 22.8 mmol) at RT for 15 mm and then iodomethane (1.42 mE,22.8 mmol) was added. The mixture was stirred for overnight, concentrated, taken into 200 mE EtOAc, washed with water x2, dried, concentrated, and subjected to silica flash colunm using 0 to 5% EtOAc in DCM to isolate the methylation product as an oil. It was treated with 1:1 TFADCM (10 mE/lO mE) at RT for 3 hours, concentrated in vacuo, taken into 200 mE EtAOc and SOmE iN NaOH. The organic phase was separated, washed with water, dried, subjected to silica flash column with 1% MeOH in DCM to isolate 3-chloro-N- methyl-5-(trifluoromethyl)aniline (467, 1.76 g, 53%) as an oil.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; JIA, Zhaozhong J.; CHEN, Wei; THOMAS, William D.; US2015/158865; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics