Continuously updated synthesis method about 367-22-6

According to the analysis of related databases, 367-22-6, the application of this compound in the production field has become more and more popular.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 367-22-6, name is 4-Chloro-3-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., Formula: C6H5ClFN

Compound 102[00318] 4-Chloro-3-fluoroaniline; (250.3g, 1.719mol) was added to a 5L four-neck round bottom flask equipped with overhead stirrer, reflux condenser, heating mantle, temperature controller, an internal temperature probe and an argon inlet. r°-Heptane (2000ml) and di-t- butyl-dicarbonate (450.3g, 2.064mol) were charged to the flask. The mixture was stirred under argon at room temperature for 15min allowing dissolution of the majority of the solids. The mixture was heated to reflux for 4h under argon (care: generation of CO2 g). Analysis of the reaction mixture by HPLC method Test 20 (THFrMeCN 1 :1) indicated complete conversion of starting material (Rt 4.57min) to one product (Rt 6.17min). [00319] The reaction was allowed to cool to 50-550C and transferred in two portions to a 3 L one-neck RBF. A total of 1500ml of distillate was removed by concentration in vacuo at 450C to give a peach colored solution with white crystals. The slurry was allowed to cool to room temperature, whilst stirring, for 1.5h. The flask was stored at 40C for 15h after which time the crystals were filtered under vacuum and washed with cold «-heptane (400ml). [00320] After drying at 350C under vacuum for 7h, very fine, white crystals of Compound 102 (393.1g, 93% yield) were obtained. Compound 102: C?Hi3ClFNO2 245.68gmol”. HPLC analysis (Test 20, MeCN): R1 6.16min; 99% purity (at) 254nm. m.p.: 103-1040C. 1H NMR OH (400 MHz, CDCl3): 1.51 (9H, s, 3 x CH3), 6.56 (IH, br-s, N-H), 6.94, 7.25, 7.35 (3 x 1Eta, 3 x m, 3 x Ar-H).

According to the analysis of related databases, 367-22-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; IDENIX PHARMACEUTICALS, INC.; WO2008/42240; (2008); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics