Réaction #302920

Équation de réaction

ethyl chloroformate

3-amino-thiophene-2-carboxylic acid methyl ester

K2CO3

→

desired product

Rendement 98.4%

3-Ethoxycarbonylamino-thiophene-2-carboxylic acid methyl ester

Rendement 98.4%

Solvants

benzene

Conditions de réaction

Traitement

1. 1
   TempératureAfter heating
2. 2
   Températureat reflux for 12 h
3. 3
   Filtrationthe mixture was filtered
4. 4
   Concentrationthe filtrate was concentrated

Mode opératoire

To a solution of 3-amino-thiophene-2-carboxylic acid methyl ester (2.39 g, 15.2 mmol) in benzene (51 mL) was added K2CO3 (6.30 g, 45.6 mmol) followed by ethyl chloroformate (1.74 mL, 18.2 mmol). After heating at reflux for 12 h, the mixture was filtered and the filtrate was concentrated to afford the desired product (3.43 g), which was used in the next step without further purification. MS: 230.0. 1H NMR (400 MHz, CD3OD) δ ppm 7.82 (d, J=5.5 Hz, 1H), 7.66 (d, J=5.6 Hz, 1H), 4.23 (q, J=7.1 Hz, 2H), 3.86 (s, 3H), 1.32 (t, J=7.1 Hz, 3H).

Source