反応 #502105

反応方程式

2-bromoisonicotinic acid

N,O-dimethylhydroxylamine hydrochloride

1-(3-dimethylaminopropyl)-3-ethyl-carbodiimide

pyridine

→

compound

収率 82.4%

2-Bromo-N-methoxy-N-methylisonicotinamide

収率 82.4%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   濃縮The mixture is concentrated
2. 2
   洗浄The organic phase is washed with 50 ml of a 1N solution of sodium hydroxide and 50 ml of a saturated solution of sodium chloride
3. 3
   乾燥dried over magnesium sulphate
4. 4
   濃縮concentrated under reduced pressure

実験手順

In a round-bottomed flask, 2.0 g of 2-bromoisonicotinic acid, 1.1 g of N,O-dimethylhydroxylamine hydrochloride, 3.8 g of 1-(3-dimethylaminopropyl)-3-ethyl-carbodiimide and 3.2 ml of pyridine are placed in 50 ml of tetrahydrofuran. The mixture is stirred at ambient temperature for 40 h. The mixture is concentrated, and the residue is taken up in 50 ml of ethyl acetate and 50 ml of water. The organic phase is washed with 50 ml of a 1N solution of sodium hydroxide and 50 ml of a saturated solution of sodium chloride, dried over magnesium sulphate and then concentrated under reduced pressure. 2.0 g of compound are obtained.

出典