ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Water → 1-(2-Nitro-vinyl)-4-trifluoromethyl-benzene

HRID 856065
ノート
印刷プレビュー

反応式

HRID 856065 の反応式
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:10]=[CH:9][C:6]([CH:7]=O)=[CH:5][CH:4]=1.C([O-])(=O)C.[NH4+].O.[N+:19]([CH3:22])([O-:21])=[O:20]>>[N+:19]([CH:22]=[CH:7][C:6]1[CH:9]=[CH:10][C:3]([C:2]([F:12])([F:11])[F:1])=[CH:4][CH:5]=1)([O-:21])=[O:20]
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 4

HCID 962WaterHCID 6375NitromethaneHCID 679964-(Trifluoromethyl)benzaldehydeHCID 517165Ammonium Acetate

生成物 1

HCID 6882311-(2-Nitro-vinyl)-4-trifluoromethyl-benzene収率 43%

実験手順

4-Trifluoromethylbenzaldehyde (3.00 g, 17.2 mmol) was dissolved in nitromethane (10 ml), to which ammonium acetate (1.341 g, 17.4 mmol) was added, and the mixture was heated under reflux for 2 hours. Water was added to the mixture, which was extracted with methylene chloride twice, and the extracts were combined and washed with brine, and dried over magnesium sulfate, and then filtered. The filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=9/1) to afford 1-(2-nitrovinyl)-4-trifluoromethylbenzene (1.596 g, yield 43%) as a pale yellow crystalline powder.

後処理

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 2 hours
  4. extractionwas extracted with methylene chloride twice
  5. washwashed with brine
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=9/1)

出典と根拠

ORDレコード
ord-fe3ce31e5205424b8175d840562729bc
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07262212B2

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