반응 #2254179

반응 방정식

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

수율 51.2%

용매

acetone

반응 조건

후처리

1. 1
   기타one night at room temperature, the reaction is quenched with water
2. 2
   추출The reaction mixture is extracted three times with ethyl acetate
3. 3
   건조The combined organic phases are dried over Na2SO4
4. 4
   농축concentrated in vacuo
5. 5
   기타The crude product is purified on a semi-preparative HPLC

실험 절차

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.

출처