反応 #2254179

反応方程式

HCl

5-[1,3]dioxolan-2-yl-3-methyl-thiophene-2-carboxylic acid (2,2,2-trifluoro-ethyl)-amide

→

5-formyl-3-methyl-thiophene-2-carboxylic acid (2,2,2-trifluoro-ethyl)-amide

収率 51.2%

溶媒

acetone

反応条件

後処理

1. 1
   その他one night at room temperature, the reaction is quenched with water
2. 2
   抽出The reaction mixture is extracted three times with ethyl acetate
3. 3
   乾燥The combined organic phases are dried over Na2SO4
4. 4
   濃縮concentrated in vacuo
5. 5
   その他The crude product is purified on a semi-preparative HPLC

実験手順

HCl (2N, 4 ml) is added to a solution of 5-[1,3]dioxolan-2-yl-3-methyl-thiophene-2-carboxylic acid (2,2,2-trifluoro-ethyl)-amide (450 mg) in acetone (10 ml). After 4 hours at 50° C. and one night at room temperature, the reaction is quenched with water. The reaction mixture is extracted three times with ethyl acetate. The combined organic phases are dried over Na2SO4 and concentrated in vacuo. The crude product is purified on a semi-preparative HPLC to yield 5-formyl-3-methyl-thiophene-2-carboxylic acid (2,2,2-trifluoro-ethyl)-amide (196 mg) as a yellowish oil. MS (HPLC/MS): 252 (MH+). Retention time: 2.54 min.

出典