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Water → HCID 19365532、化合物

HRID 849935
ノート
印刷プレビュー

反応式

HRID 849935 の反応式
O.[Cl:2][C:3]1[C:8]([N+:9]([O-])=O)=[CH:7][C:6]([C:12]2[C:13](=[O:23])[N:14]([CH3:22])[C:15]([C:18]([F:21])([F:20])[F:19])=[CH:16][N:17]=2)=[C:5]([F:24])[CH:4]=1>C(O)(=O)C.[Fe]>[NH2:9][C:8]1[C:3]([Cl:2])=[CH:4][C:5]([F:24])=[C:6]([C:12]2[C:13](=[O:23])[N:14]([CH3:22])[C:15]([C:18]([F:21])([F:20])[F:19])=[CH:16][N:17]=2)[CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 962Water2 回HCID 19365540HCID 19365540、化合物2 回

生成物 1

HCID 19365532HCID 19365532、化合物収率 46%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 176Acetic Acid溶媒2 回

実験手順

Then, 0.37 g of iron powder was added to a mixture of 5.3 ml of acetic acid and 2.0 ml of water, to which a solution of 0.39 g of 3-(4-chloro-2-fluoro-5-nitrophenyl)-1-methyl-6-trifluoromethyl-2-oxo-1,2-dihydropyrazine (present compound 1-17) in 1.0 ml of acetic acid was slowly added dropwise, and the mixture was stirred at room temperature for 3.5 hours. After completion of the reaction, the reaction mixture was poured into water, followed by extraction with ethyl acetate. The organic layer was washed twice with water and further with saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated, which afforded 0.16 g (yield, 46%) of 3-(5-amino-4-chloro-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2-oxo-1,2-dihydropyrazine (present compound 1-23).

後処理

  1. additionwas slowly added dropwise
  2. customAfter completion of the reaction
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe organic layer was washed twice with water and further with saturated sodium chloride solution
  5. dry with materialdried with anhydrous magnesium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-52eade3fa3c248bc8d8b9c9721da0a4b
出典データセット
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06015774

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート