Water → HCID 18466625、化合物

HRID 2229306ノート

反応式

HRID 2229306 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:9](Cl)=[O:10])[C:5]([Cl:8])=[N:6][CH:7]=1.[NH2:12][C:13]1[C:14]([NH:20][CH2:21][CH3:22])=[N:15][C:16]([Cl:19])=[CH:17][CH:18]=1.C([O-])(O)=O.[Na+].O>CC#N>[Br:1][C:2]1[CH:3]=[C:4]([C:9]([NH:12][C:13]2[C:14]([NH:20][CH2:21][CH3:22])=[N:15][C:16]([Cl:19])=[CH:17][CH:18]=2)=[O:10])[C:5]([Cl:8])=[N:6][CH:7]=1

参加物

6

実験手順

A solution of 5-bromo-2-chloro-3-pyridinecarbonyl chloride (30.0 g, 97.0 mmol) in MeCN (100 mL) was added via cannula to a solution of 3-amino-6-chloro-2-(ethylamino)pyridine (16.6 g, 97.0 mmol) in MeCN (180 mL) containing solid NaHCO3 (14.2 g, 169 mmol) at room temperature. The mixture was stirred at room temperature for 1 h. Water (200 mL) was added and the mixture was stirred for 10 min. The resulting suspension was filtered. The solid was washed with Et2O (50 mL) and concentrated from pyridine solution (3×50 mL) to give the title compound (28.4 g, 75% yield).

後処理

  1. stirringthe mixture was stirred for 10 min
  2. filtrationThe resulting suspension was filtered
  3. washThe solid was washed with Et2O (50 mL)
  4. concentrationconcentrated from pyridine solution (3×50 mL)

出典と根拠

ORDレコード
ord-1f98b504cb8a4793ab3cab7d384dd18a
出典データセット
uspto-grants-2002_07
特許番号
US06420359B1

反応ノート

読み込み中…