反応 #2389084

反応方程式

5-Methyl-2-thiophenecarbaldehyde

hydroxylamine hydrochloride

sodium acetate

→

5-methyl-2-thiophenecarboxamide

収率 82.0%

溶媒

acetic acid

反応条件

後処理

1. 1
   濃縮the reaction mixture was concentrated under reduced pressure to about one-half of its volume
2. 2
   workup.ADDITIONTo this concentrate was added concentrated hydrochloric acid (100 ml)
3. 3
   workup.ADDITIONThe reaction mixture was then diluted with 100 ml of water
4. 4
   温度cooling for 30 minutes
5. 5
   ろ過The resulting crystals were recovered by filtration
6. 6
   洗浄rinsed with 100 ml of iced water

実験手順

5-Methyl-2-thiophenecarbaldehyde (2.6 g, 0.1 M), hydroxylamine hydrochloride (8.3 g, 0.12 M), and sodium acetate (9.8 g, 0.12 M) were added to. acetic acid (50 ml) and the mixture was refluxed for 13 to 15 hours. After disappearance of the starting material was confirmed by high performance liquid chromatography (HPLC retention time ca 13 min.), the reaction mixture was concentrated under reduced pressure to about one-half of its volume. To this concentrate was added concentrated hydrochloric acid (100 ml) and the reaction was allowed to proceed at 60° C. for 4 hours. The reaction mixture was then diluted with 100 ml of water and stirred under ice-cooling for 30 minutes. The resulting crystals were recovered by filtration and rinsed with 100 ml of iced water to provide 5-methyl-2-thiophenecarboxamide (HPLC retention time ca 4 min.)

出典