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. 68322-84-9, name is 2-Bromo-1-fluoro-4-(trifluoromethyl)benzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 68322-84-9
3-Bromo-4-fluorobenzotrifluoride (0.38 mL, 2.67 mmol), Cs2C03 (1.74 g, 5.34 mmol), X-Phos (207 mg, 0.036 mmol) and Pd2(dba)3 (164 mg, 0.18 mmol), were added to a mixture of intermediate 31 and intermediate 32 (510 mg, 1.78 mmol) in 2-methyl-2- propanol (40 mL) under a N2 atmosphere. The r.m. was heated at 100 C for 16 h. Then, the r.m. was cooled to r.t., water was added and the r.m. was extracted with DCM. The combined organic layers were dried (MgS04), filtered and concentrated in vacuo. The residue was purified by flash column chromatography (eluent: DCM/MeOH from 100/0 to 95/5). The product fractions were collected and concentrated in vacuo. Both residue was suspended in DIPE and treated with a 6 N HC1 sol. in 2-propanol. Resulting precipitates were collected by filtration. The first compound impure was repurified by RP preparative HPLC [RP Vydac Denali CI 8 – IotaOmicronmu?iota, 250 g, 5cm); mobile phase: a gradient of (0.25% H4HC03 sol. in water/CH3CN)]. The product fractions were collected and concentrated in vacuo. Both residue was crystallized from DIPE, filtered off and dried. Yield: 118 mg of compound 11 (13 %) as HC1 salt (.HC1 .H20) and 97 mg of compound 11a (12 %; regioisomer of compound 11).
The synthetic route of 68322-84-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; JANSSEN PHARMACEUTICALS, INC.; BISCHOFF, Francois, Paul; VELTER, Adriana, Ingrid; VAN BRANDT, Sven, Franciscus, Anna; BERTHELOT, Didier, Jean-Claude; WO2012/126984; (2012); A1;,
Bromide – Wikipedia,
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