Pyridine → 6-Chloro-2-(ethylamino)pyridine-3-carbonyl fluoride

HRID 2207305ノート

反応式

HRID 2207305 の反応式
N1C=CC=CC=1.[F:7]N1N=C(F)C=C(F)N1.[Cl:16][C:17]1[CH:25]=[CH:24][C:20]([C:21](O)=[O:22])=[C:19]([NH:26][CH2:27][CH3:28])[N:18]=1>ClCCl>[Cl:16][C:17]1[CH:25]=[CH:24][C:20]([C:21]([F:7])=[O:22])=[C:19]([NH:26][CH2:27][CH3:28])[N:18]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 216944332,4,6-Trifluoro-1,2,3-triazineHCID 633764796-Chloro-2-(ethylamino)nicotinic acid

生成物 1

HCID 867145746-Chloro-2-(ethylamino)pyridine-3-carbonyl fluoride収率 99.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2 ml (24.8 mmol) of pyridine and 4.2 ml (49.8 mmol) of 2,4,6-trifluorotriazine were added to a suspension of 5.0 g (24.8 mmol) of 6-chloro-2-ethylamino-nicotinic acid in 125 ml of dichloromethane. The mixture was stirred for 3 hours at ambient temperature and then filtered. The solid was rinsed with 50 ml of dichloromethane and the filtrate was washed twice with 60 ml of ice-cold water. The organic phase was dried over Na2SO4 and the solvent was evaporated off under reduced pressure. 5.01 g of product were obtained in the form of an orange oil which was used without further purification.

後処理

  1. filtrationfiltered
  2. washThe solid was rinsed with 50 ml of dichloromethane
  3. washthe filtrate was washed twice with 60 ml of ice-cold water
  4. dry with materialThe organic phase was dried over Na2SO4
  5. customthe solvent was evaporated off under reduced pressure

出典と根拠

ORDレコード
ord-892b107875144d8fb9d2bc4c30046293
出典データセット
uspto-grants-2016_06
特許番号
US09376432B2

反応ノート

読み込み中…