反応 #79047

反応方程式

6-chloro-3-nitropicolinamide

→

3-amino-6-chloropicolinamide

溶媒

EtOAc

反応条件

後処理

1. 1
   その他After removal of the catalyst
2. 2
   ろ過by filtration the solution
3. 3
   濃縮is concentrated to dryness

実験手順

A solution of 6-chloro-3-nitropicolinamide (0.30 g, 1.49 mmol) in EtOAc (30 mL) is hydrogenated at 60 psi over 5% Pd-C (0.10 g) for 20 min. After removal of the catalyst by filtration the solution is concentrated to dryness to give 3-amino-6-chloropicolinamide as a yellow oil, which is used directly in the next step. It is dissolved in triethylorthoformate (30 mL) and the mixture is heated under reflux for 18 h. Petroleum ether (30 mL) is added to the cooled solution, and the resulting precipitate of crude 6-chloro-3H-pyrido[3,2-d]pyrimidin-4-one (0.27 g, 99%) is filtered off and dried in a vacuum oven.

出典