Reaktion #502105

Reaktionsgleichung

2-bromoisonicotinic acid

N,O-dimethylhydroxylamine hydrochloride

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

pyridine

→

compound

Ausbeute 82.4%

2-Bromo-N-methoxy-N-methylisonicotinamide

Ausbeute 82.4%

Lösungsmittel

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe mixture is concentrated
2. 2
   WaschenThe 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
   Trocknendried over magnesium sulphate
4. 4
   Einengenconcentrated under reduced pressure

Vorschrift

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.

Quelle