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Nitric Acid → HCID 68986110、化合物

HRID 1930304
ノート
印刷プレビュー

反応式

HRID 1930304 の反応式
[N+:1]([O-:4])(O)=[O:2].[Br:5][C:6]1[CH:11]=[C:10]([F:12])[CH:9]=[CH:8][C:7]=1[CH2:13][C:14]([OH:16])=[O:15]>>[Br:5][C:6]1[CH:11]=[C:10]([F:12])[C:9]([N+:1]([O-:4])=[O:2])=[CH:8][C:7]=1[CH2:13][C:14]([OH:16])=[O:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 944Nitric AcidHCID 34778092-Bromo-4-fluorophenylacetic acid

生成物 1

HCID 68986110HCID 68986110、化合物収率 51%

実験手順

To stirring fuming HNO3 (15 mL) at −15° C. was added 2-bromo-4-fluorophenylacetic acid (10 g, 43 mmol) in portions such that the internal temperature remained below −10° C. After completing the addition the reaction was stirred with warming to +5° C. over 15 min. The mixture was poured onto ice (500 g). Product separated as a slightly sticky solid which on manipulation with a spatula became powdery. The suspension was stirred vigorously until the ice had completely melted. While still very cold, the solids were collected by filtration, rinsed very well with H2O (1 L). The solid was dried under vacuum to afford 2-(2-bromo-4-fluoro-5-nitrophenyl)acetic acid (6.04 g, 51% yield) as a pale yellow solid which was used as is in the next reaction.

後処理

  1. customremained below −10° C
  2. additionthe addition the reaction
  • temperaturewith warming to +5° C. over 15 min
  • additionThe mixture was poured onto ice (500 g)
  • customProduct separated as a slightly sticky solid which on manipulation with a spatula
  • stirringThe suspension was stirred vigorously until the ice
  • filtrationWhile still very cold, the solids were collected by filtration
  • washrinsed very well with H2O (1 L)
  • customThe solid was dried under vacuum
  • 出典と根拠

    ORDレコード
    ord-368ac0e827be489a85bcb779f3b7135f
    出典データセット
    uspto-grants-2012_05
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US08188113B2

    反応ノート

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