反应详情

To a solution of 30.0 g of 4,5,6,7-tetrahydro-4-oxo-3-benzofurancarboxylic acid in 225 ml of ethanol is added 22.97 g of hydroxylamine hydrochloride, followed by 18.10 g of sodium acetate and 55 ml of water. The reaction mixture is heated at reflux for 2.5 hours and concentrated in vacuo to a residue which is diluted with 600 ml of ethyl acetate, washed with 2×200 ml of water, brine and dried over Na2SO4. The organic layer is concentrated in vacuo to a residue which is dried under vacuum to give 31.0 g of the desired product as a solid.

1. temperatureThe reaction mixture is heated
2. temperatureat reflux for 2.5 hours
3. concentrationconcentrated in vacuo to a residue which
4. additionis diluted with 600 ml of ethyl acetate
5. washwashed with 2×200 ml of water, brine
6. dry with materialdried over Na2SO4
7. concentrationThe organic layer is concentrated in vacuo to a residue which
8. customis dried under vacuum