p-Fluoronitrobenzene → N-(4-Nitrophenyl)pyridin-2-amine

HRID 2054105ノート

反応式

HRID 2054105 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=1.[NH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=1.C([O-])([O-])=O.[K+].[K+].CC(C)([O-])C.[K+]>O.CN1CCCC1=O>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([NH:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=2)=[CH:3][CH:4]=1)([O-:10])=[O:9]

参加物

7

反応物 4

HCID 9590p-FluoronitrobenzeneHCID 104392-AminopyridineHCID 11430Potassium CarbonateHCID 23665647Potassium tert-butoxide

生成物 1

HCID 12695755N-(4-Nitrophenyl)pyridin-2-amine収率 19.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
60 °C

実験手順

0.3 g of 4-fluoronitrobenzene, 0.4 g of 2-aminopyridine, and 0.353 g of K2CO3 were added to a solution of 2.5 ml of N-methylpyrrolidinone. The reaction medium was heated at 60° C. for 1 hour and 0.286 g of potassium tert-butoxide was then added. Heating was then continued for 6 hours and, after cooling to room temperature, the reaction medium was then poured into a water and ice mixture. The yellow precipitate formed was filtered off, reslurried in water and then dried over P2O5. 0.09 g of N-(4-nitrophenyl)pyrid-2-amine (5) was obtained.

後処理

  1. temperatureHeating
  2. temperatureafter cooling to room temperature
  3. customThe yellow precipitate formed
  4. filtrationwas filtered off
  5. dry with materialdried over P2O5

出典と根拠

ORDレコード
ord-04b152c713f746bd990f3f61d0b4e626
出典データセット
uspto-grants-2008_02
特許番号
US07329288B2

反応ノート

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