These common heterocyclic compound, 22236-08-4, name is 3-(Difluoromethoxy)aniline, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Quality Control of 3-(Difluoromethoxy)aniline
A solution of 4-chloro-6-nitro-2- (pyrazin-2-yl) quinazoline (1.00 g, crude, 3.7 mmol, 1.0 equiv), 3- (difluoromethoxy) benzenamine 600 mg, 3.7 mmol, 1.0 eq) and Et 3 N (1.00 g, 10 mmol, 3.0 eq) was stirred at 75 C. for 18 h. After cooling, the volatiles were removed in vacuo and the residue was washed with H 2 O (100 mL × 2). The solid was dried in vacuo to give 1.40 g of N- (3- (difluoromethoxy) phenyl) -6-nitro-2- (pyrazin-2-yl) quinazolin-4-amine as a black solid 90.2% at the stage). LCMS m / z = 411.0 (M + 1) (Method A) (retention time = 1.61 min).
The synthetic route of 3-(Difluoromethoxy)aniline has been constantly updated, and we look forward to future research findings.
Reference:
Patent; OTSUKA PHARMACEUTICAL COMPANY LIMITED; SUZUKI, MASAKI; KONDO, KAZUMI; KURIMURA, MUNEAKI; VALLURU, KRISHNA REDDY; TAKAHASHI, AKIRA; KURODA, TAKESHI; TAKAHASHI, HARUKA; FUKUSHIMA, TAE; MIYAMURA, SHIN; GHOSH, INDRANATH; DOGRA, ABHISHEK; HARRIMAN, GERALDINE; ELDER, AMY; SHIMIZU, SATOSHI; HODGETTS, KEVIN J; NEWCOM, JASON S; (678 pag.)JP6121658; (2017); B2;,
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