3-(NITROMETHYL)-2-BENZOFURAN-1(3H)-ONE synthesis
- Product Name:3-(NITROMETHYL)-2-BENZOFURAN-1(3H)-ONE
- CAS Number:3598-68-3
- Molecular formula:C9H7NO4
- Molecular Weight:193.16
Yield:3598-68-3 100%
Reaction Conditions:
with sodium hydroxide in methanol at 15 - 30; for 1 h;
Steps:
1.a
Compound 1 (50 g, 0.33 mol) and nitromethane (44 mL, 0.80 mol) were dissolved in methanol (400 mL) and a solution of sodium hydroxide (5M- 15M, 100 mL).The reaction was stirred at 15 °C to 30 °C for 1 hour. TLC (petroleum ether / ethyl acetate = 2: 1, volume ratio, the same below) showed that the reaction was completed. The reaction system was added dropwise aq. HCl (4M-8M, 800 mL) at 10 ° C to 20 ° C. The reaction system was cooled to 5 to 10 , a large number of white solid precipitation, collected by filtration, washed with a small amount of water, placed in a vacuum oven to dry, Compound 2 (64 g) was obtained as a white solid in 100% yield.
References:
CN105884762,2016,A Location in patent:Paragraph 0006
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