反应详情

温度

60 °C

NMR Method for hydrocarboxylation product sample analysis. DCl/D2O/propionic acid stock solution preparation: D2O (99.99%, CIL) (74.606 g), 35% DCl in D2O (CIL) (47.755 g) and propionic acid (JT Baker) (2.198 g) were thoroughly mixed in a bottle to give 0.01765 g of propionic acid per g of stock solution. Hydrocarboxylation product sample preparation for 1H NMR analysis: About 50 mg of hydrocarboxylation sample was transferred to a 2 dram screw top vial with a phenolic cap with a polypropylene liner and the exact mass of the sample was recorded. Then 0.8288 g of stock solution was added and the mixture was heated in a heat block for 1 hour at 60° C. The vial was allowed to cool to room temperature and then the solution was transferred to an NMR tube. 1H NMR analysis: 1H NMR was recorded using 30 seconds pulse delay, 90 degree pulse angle, 16 scans and D2O lock solvent. The spectrum was referenced to the CH3 triplet of propionic acid (1.15 ppm). The meq/g concentrations of the following components were obtained from peak integrations (A1 δ 8.36 ppm, F0 δ 4.99, 4.94 ppm, MeOCH2OH δ 4.83 ppm, MGH δ 3.52 ppm, MG δ 3.84 ppm, MGM δ 3.85 ppm, G1 δ 4.35 ppm, MeOH δ 3.47 ppm, MeOPr (methyl propionate) δ 3.76 ppm, HOPr (ISTD) δ 2.50 ppm).

1. customHydrocarboxylation product sample preparation for 1H NMR analysis
2. additionThen 0.8288 g of stock solution was added
3. temperatureto cool to room temperature
4. customthe solution was transferred to an NMR tube
5. custompulse delay, 90 degree pulse angle, 16 scans and D2O