p-Methoxy-N,N-dimethylbenzamide synthesis
- Product Name:p-Methoxy-N,N-dimethylbenzamide
- CAS Number:7291-00-1
- Molecular formula:C10H13NO2
- Molecular Weight:179.22
Yield:7291-00-1 98%
Reaction Conditions:
with oxygen;sodium hydroxide in water at 25; for 24 h;
Steps:
General procedure for the amidation using Au/HAP catalyst
General procedure: Unless otherwise noted, reactions were carried out as following: a mixture of alcohol 1 (1.00mmol, 2.0 equiv), amine 2 (0.50 mmol), sodium hydroxide (0.50 mmol) and Au/HAP (45 mg, 1.69wt%) were vigorously stirred in 0.5 mL H2O at 40 °C for 24 h under oxygen balloon. After completion of the reaction, the mixture is cooled to room temperature, diluted with ethyl acetate. The catalyst was separated by centrifugation and washed with ethyl acetate (3 x 15.0 mL). The combined organic layer was washed by saturated NaCl solution and dried over anhydrous magnesium sulfate and the solvent was removed under vacuum. The residue was purified by flash chromatography on a short silica gel (eluent: petroleum ether/ethyl acetate = 10:1, 2:1, or 1:1) toafford the corresponding amide 3.
References:
Wang, Wentao;Cong, Yu;Zhang, Leilei;Huang, Yanqiang;Wang, Xiaodong;Zhang, Tao [Tetrahedron Letters,2014,vol. 55,# 1,p. 124 - 127] Location in patent:supporting information
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