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4-Amino-2-(trifluoromethyl)benzonitrile → HCID 11246104、化合物

HRID 982665
ノート
印刷プレビュー

反応式

HRID 982665 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7]1[C:8](=[O:14])O[C:10](=[O:13])[C:11]=1[CH3:12].[NH2:15][C:16]1[CH:23]=[CH:22][C:19]([C:20]#[N:21])=[C:18]([C:24]([F:27])([F:26])[F:25])[CH:17]=1>C(O)C>[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7]1[C:8](=[O:14])[N:15]([C:16]2[CH:23]=[CH:22][C:19]([C:20]#[N:21])=[C:18]([C:24]([F:25])([F:26])[F:27])[CH:17]=2)[C:10](=[O:13])[C:11]=1[CH3:12]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 5221704-Amino-2-(trifluoromethyl)benzonitrileHCID 113789433-(5-Chloropentyl)-4-methyl-2,5-furandione

生成物 1

HCID 11246104HCID 11246104、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
90 °C

実験手順

A mixture of 9.46 g of 3-(5-chloropentyl)-4-methyl-2,5-furandione and 8.13 g of 4-amino-2-(trifluoromethyl)benzonitrile in 22 ml of ethanol was mixed under a nitrogen atmosphere with 2.5 g of an activated molecular sieve (0.3 nm), and it was stirred for 2 days at 90° C. For working-up, the molecular sieve was filtered off after cooling, washed with ethanol, and the combined ethanol solutions were concentrated by evaporation. The residue was taken up in ethyl acetate and washed with water as well as saturated sodium chloride solution. After drying on sodium sulfate and concentration by evaporation, it was chromatographed on silica gel with ethyl acetate/hexane/toluene, and 11.69 g of the title compound was thus obtained as a white solid.

後処理

  1. additionwas mixed under a nitrogen atmosphere with 2.5 g of an activated molecular sieve (0.3 nm), and it
  2. filtrationthe molecular sieve was filtered off
  3. temperatureafter cooling
  4. washwashed with ethanol
  5. concentrationthe combined ethanol solutions were concentrated by evaporation
  6. washwashed with water as well as saturated sodium chloride solution
  7. customAfter drying on sodium sulfate and concentration by evaporation, it
  8. customwas chromatographed on silica gel with ethyl acetate/hexane/toluene, and 11.69 g of the title compound
  9. customwas thus obtained as a white solid

出典と根拠

ORDレコード
ord-4a049e2a72a5434eb0e8de77a4fe005e
出典データセット
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06861432B2

反応ノート

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