反应详情

温度

65 °C

α-Amino(2,3-dihydro-5-benzofuranyl)acetic acid (200 mg, 1.04 mmole) is dissolved in 250 mg (4.14 mmole) of glacial acetic acid and 145 mg (2.08 mmole) of sodium nitrite in about 5 ml of water is added dropwise. An additional 1 ml of glacial acetic acid is added and the mixture is heated to 65° C. and held at 65° C. for 4 hours. After cooling the reaction mixture is diluted with water and extracted with ethyl acetate for several hours. The ethyl acetate is dried over magnesium sulfate, filtered and evaporated to give a 65% yield of the title compound. NMR(DMSO-D6)ppm(δ)7.15(m,3); 5.18(d,1); 4.78(t,2) and 3.34(t,2).

1. temperatureAfter cooling the reaction mixture
2. extractionextracted with ethyl acetate for several hours
3. dry with materialThe ethyl acetate is dried over magnesium sulfate
4. filtrationfiltered
5. customevaporated