تفاعل #2254179

معادلة التفاعل

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

المردود 51.2%

المذيبات

acetone

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر