Electric Literature of 208511-67-5,Some common heterocyclic compound, 208511-67-5, name is 4-(1H-Pyrazol-3-yl)benzoic acid, molecular formula is C10H8N2O2, 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.
General procedure: The following compounds were made in a parallel manner using the following procedure: Reauents were weighed into stubby tubes. Stock solutions were made for reagent addition : Dissolved 2305.8 mg Intermediate 4 in 45.75 niL DMF and DIEA(2 eq). Dissolved 3131.85 mg HATU in 75 mE DMF. To each vial containing reagent acid(0.063 mmoi) was added 0.25 ml of the HAT1 solution in DMF followed by DIEA (0.028 mL, 0.158 mrnoi). After stirring for 10 mm, 0.25 ml of the intermediate 4 solution was added and the resulting reaction mixture vials were placed in a Bohdan Miniblock XT and were agitated overnight at 400rpm.Upon completion, reaction mixtures were purified via preparative LC/MS with thefollowing conditions: Column: XBridge C18, 19 x 100 mm, 5-.tm particles; Mobile PhaseA: 5:95 acetonitrile: water with 10 ml?I ammoniumn acetate; Mobile Phase B: c.5:5 acetonitrile: water with 10 m?1 ammonium acetate; Gradient: 10-50% B over 20 minutes, then a 2-minute hold at 100% B; Flow: 20 mL/min. Fractions containing the desired product were combined and dmied via centrifugal evaporation. **Gradient varied for eachreaction depending on polarity of comnpound.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-(1H-Pyrazol-3-yl)benzoic acid, its application will become more common.