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Acetic Acid → N2-(2,2,2-trifluoroethyl)-5-trifluoromethylpyridine-2,3-diamine

HRID 1477306
ノート
印刷プレビュー

反応式

HRID 1477306 の反応式
O.C(O)(=O)C.[N+:6]([C:9]1[C:10]([NH:19][CH2:20][C:21]([F:24])([F:23])[F:22])=[N:11][CH:12]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:14]=1)([O-])=O>[Fe].C(O)C>[F:24][C:21]([F:22])([F:23])[CH2:20][NH:19][C:10]1[C:9]([NH2:6])=[CH:14][C:13]([C:15]([F:16])([F:17])[F:18])=[CH:12][N:11]=1
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

6

反応物 3

HCID 176Acetic AcidHCID 962WaterHCID 86725178(3-Nitro-5-trifluoromethylpyridin-2-yl)-(2,2,2-trifluoroethyl)amine

生成物 1

HCID 86725179N2-(2,2,2-trifluoroethyl)-5-trifluoromethylpyridine-2,3-diamine収率 96.9%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 702
Ethanol
溶媒
2 回

反応条件

温度
70 °C

実験手順

A mixture of an iron powder (2.12 g), ethanol 6 ml), water 4 ml) and acetic acid 0.1 ml) was added dropwise a mixture of (3-nitro-5-trifluoromethylpyridin-2-yl)-(2,2,2-trifluoroethyl)amine (1.83 g) and ethanol (10 ml) at 70° C., and then the mixture was stirred at 70° C. for 1 hour. After allowing to cool, the cooled reaction mixture was filtrated. To the filtrate was added water, and then the mixture was extracted with ethyl acetate. The organic layer was washed with water, dried over sodium sulfate, and concentrated under reduced pressure to give N2-(2,2,2-trifluoroethyl)-5-trifluoromethylpyridin-2,3-diamine (1.59 g).

後処理

  1. additionwas added dropwise
  2. temperatureto cool
  3. customthe cooled reaction mixture
  4. filtrationwas filtrated
  5. additionTo the filtrate was added water
  6. extractionthe mixture was extracted with ethyl acetate
  7. washThe organic layer was washed with water
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-12e41fe0f68845928d4e53325513b789
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09403771B2

反応ノート

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