Synthetic Route of 90267-03-1, These common heterocyclic compound, 90267-03-1, name is 1-Bromo-3,5-diethylbenzene, 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.
A mixture of N- ( 4- (methylsulfonyl ) benzyl ) -2 , 3 , 4 , 5- tetrahydro-1 , 5-benzoxazepine-8-carboxamide (29 mg, 0.08 mmol), l-bromo-3, 5-diethylbenzene (34 mg, 0.160 mmol), RuPhos-Pd-Gl (5.83 mg, 8.00 mumol) , RuPhos (3.73 mg, 8.00 mumol) , NaOtBu (23 mg, 0.240 mmol) and DME (1 mL) was heated at 130C for 2 h under microwave irradiation. The reaction mixture was diluted with AcOEt (3 mL) and quenched with H20 (1 mL) , and stirred for 2 min. The organic layer was separated and then the aqueous layer was extracted with EtOAc (2 mL) . The combined organic layer was evaporated by blowing away with the air at 60 C. The residue was purified by preparative HPLC (Actus Triart C18, eluted with MeCN/10 mM NH4HCO3 aq. 5 : 95?100 : 0 ) . Pure fractions were combined and concentrated by blowing away with the air at 60C to afford the title compound (14.4 mg, 0.0292 mmol, 37%).
The synthetic route of 90267-03-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; YAMAMOTO, Satoshi; SHIRAI, Junya; KONO, Mitsunori; SHIOKAWA, Zenyu; YUKAWA, Tomoya; IMADA, Takashi; NEGORO, Nobuyuki; ODA, Tsuneo; SASAKI, Satoshi; NARA, Yoshi; SUZUKI, Shinkichi; SATO, Ayumu; ISHII, Naoki; SHIBUYA, Akito; NAKAGAWA, Yasuo; COLE, Derek; GIBSON, Tony; IVETAC, Anthony; SWANN, Steve; TYHONAS, John; (472 pag.)WO2018/30550; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary