Triethylamine → 2-Chloro-5-fluoropyridine-3-carbonitrile

HRID 510026ノート

反応式

HRID 510026 の反応式
C(N(CC)CC)C.[Cl:8][C:9]1[N:17]=[CH:16][C:15]([F:18])=[CH:14][C:10]=1[C:11]([NH2:13])=O.FC(F)(F)C(OC(=O)C(F)(F)F)=O>ClCCl>[Cl:8][C:9]1[N:17]=[CH:16][C:15]([F:18])=[CH:14][C:10]=1[C:11]#[N:13]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 9845Trifluoroacetic anhydrideHCID 126297962-Chloro-5-fluoropyridine-3-carboxamide

生成物 1

HCID 231108512-Chloro-5-fluoropyridine-3-carbonitrile

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

81.2 ml (582.25 mmol) of triethylamine were added to a suspension of 46.2 g (264.66 mmol) of 2-chloro-5-fluoronicotinamide in dichloromethane (783 ml), and the mixture was cooled to 0° C. Then, while stirring, 41.12 ml (291.13 mmol) of trifluoroacetic anhydride were slowly added dropwise and the mixture was stirred at 0° C. for 1.5 h. The reaction solution was subsequently washed twice with saturated aqueous sodium hydrogencarbonate solution (391 ml each time), dried and concentrated under reduced pressure.

後処理

  1. stirringthe mixture was stirred at 0° C. for 1.5 h
  2. washThe reaction solution was subsequently washed twice with saturated aqueous sodium hydrogencarbonate solution (391 ml each time)
  3. customdried
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1389f5bc688941218dd67aeb143edb2c
出典データセット
uspto-grants-2015_08
特許番号
US09096592B2

反応ノート

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