反応 #450359

反応方程式

sodium hydroxide

4'-chloro-2'-fluoro-5'-[hexahydro-2,4, 6-trioxo-3-(2-propynyl)-s-triazin-1-yl]acetanilide

hydrochloric acid

ethyl acetate

→

title product

収率 82.2%

1-(5-Amino-2-chloro-4-fluorophenyl)-3 -(2-propynyl)-s-triazine-2,4,6-(1H, 3H, 5H)-trione

収率 82.2%

溶媒

ethanol

反応条件

後処理

1. 1
   温度is refluxed for 3 hours
2. 2
   その他the phases are separated
3. 3
   洗浄The organic phase is washed sequentially with saturated sodium hydrogen carbonate solution and brine
4. 4
   濃縮concentrated in vacuo

実験手順

A mixture of 4'-chloro-2'-fluoro-5'-[hexahydro-2,4, 6-trioxo-3-(2-propynyl)-s-triazin-1-yl]acetanilide (3.00 g, 8.5 mmol), and 3N hydrochloric acid (25 mL) in ethanol (50 mL) is refluxed for 3 hours, cooled to room temperature, and poured into ethyl acetate. 3N sodium hydroxide solution (25 mL) is added to the organic solution, and the phases are separated. The organic phase is washed sequentially with saturated sodium hydrogen carbonate solution and brine, and concentrated in vacuo to give the title product as a beige solid (2.17 g, mp 118°-121° C.).

出典