反応 #586110
ord-edcec835b10543288395ff8b99605f27
反応方程式
methyl 2-[2-chloro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)-4-fluoro-benzoyloxy]-2-methylpropionate
hydrochloric acid
→
2-[2-chloro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)-4-fluorobenzoyloxy]-2-methylpropionic acid
収率 68.4%
反応物
試薬
なし
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度the reaction mixture was heated
- 2温度under reflux for 5 hours
- 3workup.DISTILLATIONMost of the acetic acid was distilled off
- 4workup.ADDITIONthe solution that remained was poured into ice-water
- 5ろ過The precipitate was filtered off
- 6その他dried
実験手順
1.0 g (2.1 mmol) of methyl 2-[2-chloro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)-4-fluoro-benzoyloxy]-2-methylpropionate from example 4.1 was dissolved in 50 ml of acetic acid, 50 ml of conc. hydrochloric acid were added and the reaction mixture was heated under reflux for 5 hours. Most of the acetic acid was distilled off, and the solution that remained was poured into ice-water. The precipitate was filtered off and dried, which gave 0.65 g of 2-[2-chloro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)-4-fluorobenzoyloxy]-2-methylpropionic acid.