反応 #2026369

反応方程式

water

sodium acetate

4,5,6,7-tetrahydro-4-oxo-3-benzofurancarboxylic acid

hydroxylamine hydrochloride

→

desired product

収率 95.4%

(Z)-4,5,6,7-Tetrahydro-4-(hydroxyimino)-3-benzofurancarboxylic acid

収率 95.4%

溶媒

ethanol

反応条件

後処理

1. 1
   温度The reaction mixture is heated
2. 2
   温度at reflux for 2.5 hours
3. 3
   濃縮concentrated in vacuo to a residue which
4. 4
   workup.ADDITIONis diluted with 600 ml of ethyl acetate
5. 5
   洗浄washed with 2×200 ml of water, brine
6. 6
   乾燥dried over Na2SO4
7. 7
   濃縮The organic layer is concentrated in vacuo to a residue which
8. 8
   その他is dried under vacuum

実験手順

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.

出典