반응 #502105

ord-a83387cdb3d04fc18f5c12294af90f82

반응 방정식

O=C(O)c1ccnc(Br)c1
2-bromoisonicotinic acid
CNOC.Cl
N,O-dimethylhydroxylamine hydrochloride
CCN=C=NCCCN(C)C
1-(3-dimethylaminopropyl)-3-ethyl-carbodiimide
c1ccncc1
pyridine
CON(C)C(=O)c1ccnc(Br)c1
compound
수율 82.4%
CON(C)C(=O)c1ccnc(Br)c1
2-Bromo-N-methoxy-N-methylisonicotinamide
수율 82.4%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The mixture is concentrated
  2. 2
    세척The 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
    건조dried over magnesium sulphate
  4. 4
    농축concentrated under reduced pressure

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08088765B2uspto-grants-2012_01