反应详情

温度

100 °C

To a mixture of 4-(5-methyl-furan-2-ylmethyl)-benzaldehyde (96 mg, 0.48 mmol) described in Manufacturing Example 46-1-3 and acetic acid (1 mL) were added nitromethane (190 μL, 3.6 mmol) and ammonium acetate (110 mg, 1.4 mmol) at room temperature, which was stirred for 3 hours at 100° C. The reaction mixture was cooled to room temperature, and extracted by addition of water and ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride and dried over magnesium sulfate. The filtrate was concentrated under a reduced pressure to obtain the title compound (120 mg) as a crude product. This compound was used in the following reaction without further purification.

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionextracted by addition of water and ethyl acetate
3. washThe organic layer was washed with saturated aqueous sodium chloride
4. dry with materialdried over magnesium sulfate
5. concentrationThe filtrate was concentrated under a reduced pressure