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

HRID 536476ノート

反応式

HRID 536476 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 was added to a suspension of 46.2 g (264.66 mmol) of 2-chloro-5-fluoronicotinamide in dichloromethane (783 ml) and cooled to 0° C. While stirring, 41.12 ml (291.13 mmol) of trifluoroacetic acid anhydride was slowly added dropwise and stirred for a further 1.5 h at 0° C. The reaction solution was then washed twice with saturated aqueous sodium hydrogen carbonate solution (391 ml each time), dried and concentrated by vacuum evaporation.

後処理

  1. stirringstirred for a further 1.5 h at 0° C
  2. washThe reaction solution was then washed twice with saturated aqueous sodium hydrogen carbonate solution (391 ml each time)
  3. customdried
  4. concentrationconcentrated by vacuum evaporation

出典と根拠

ORDレコード
ord-9f1ee4999b1e41029805d4fc7eb963d2
出典データセット
uspto-grants-2014_10
特許番号
US08859569B2

反応ノート

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