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Trifluoroacetic acid → 3-Chloro-2-(4-hydroxycarbonylmethyl-3-nitrophenyl)-5-tri-fluoromethylpyridine

HRID 1276091
ノート
印刷プレビュー

反応式

HRID 1276091 の反応式
FC(F)(F)C(O)=O.[Cl:8][C:9]1[C:10]([C:19]2[CH:24]=[CH:23][C:22]([CH:25](C(OC(C)(C)C)=O)[C:26]([O:28]C(C)(C)C)=[O:27])=[C:21]([N+:40]([O-:42])=[O:41])[CH:20]=2)=[N:11][CH:12]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:14]=1>ClCCl>[Cl:8][C:9]1[C:10]([C:19]2[CH:24]=[CH:23][C:22]([CH2:25][C:26]([OH:28])=[O:27])=[C:21]([N+:40]([O-:42])=[O:41])[CH:20]=2)=[N:11][CH:12]=[C:13]([C:15]([F:17])([F:16])[F:18])[CH:14]=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

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 221148383-Chloro-2-[4-(bis-[1,1-dimethylethoxycarbonyl]methyl)-3-nitrophenyl]-5-trifluoromethylpyridine

生成物 1

HCID 221148563-Chloro-2-(4-hydroxycarbonylmethyl-3-nitrophenyl)-5-tri-fluoromethylpyridine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
23 °C

実験手順

16 ml of trifluoroacetic acid were added dropwise to a solution of 10.2 g of 3-chloro-2-[4-(bis-[1,1-dimethylethoxycarbonyl]-methyl)-3-nitrophenyl]-5-trifluoromethylpyridine in 100 ml of anhydrous dichloromethane. After stirring at 23° C. for 65 hours, the methylene chloride was removed by distillation. The residue was dissolved in 100 ml of ether, after which the ether phase was extracted three times with 50 ml of water each time, dried over sodium sulfate and concentrated. The crude product was stirred with n-hexane/ether (9:1). Yield: 5.1 g (72%) of colorless crystals.

後処理

  1. customthe methylene chloride was removed by distillation
  2. dissolutionThe residue was dissolved in 100 ml of ether
  3. extractionafter which the ether phase was extracted three times with 50 ml of water each time
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. stirringThe crude product was stirred with n-hexane/ether (9:1)

出典と根拠

ORDレコード
ord-dceb09d04ba74385bbb4da0d3dc8e8e2
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06165941

反応ノート

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