Sodium Hydroxide → HCID 178491837、化合物

HRID 1963006ノート

反応式

HRID 1963006 の反応式
[F:1][C:2]1[C:9]([O:10][CH3:11])=[CH:8][CH:7]=[C:6]([F:12])[C:3]=1[C:4]#[N:5].Cl.[NH2:14][OH:15].[OH-].[Na+]>CCO>[F:1][C:2]1[C:9]([O:10][CH3:11])=[CH:8][CH:7]=[C:6]([F:12])[C:3]=1[C:4]([NH:14][OH:15])=[NH:5]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 37918322,6-Difluoro-3-methoxybenzonitrile

生成物 1

HCID 178491837HCID 178491837、化合物収率 43.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 2,6-difluoro-3-methoxybenzonitrile (0.30 g, 1.70 mmol) in EtOH (10 ml) was added hydroxylamine hydrochloride (0.12 g, 1.70 mmol) and NaOH (0.071 g, 1.70 mmol). The resulting reaction mixture was refluxed for 15 h. After the completion of the reaction (TLC monitoring), the mixture was concentrated, added EtOH and filtered. The filtrate was evaporated in vacuo and the crude residue was purified over silica gel (60-120 M, 30% EtOAc-Hexane) to get the desired product (0.15 g, 42%) as a white solid.

後処理

  1. customThe resulting reaction mixture
  2. temperaturewas refluxed for 15 h
  3. customAfter the completion of the reaction (TLC monitoring)
  4. concentrationthe mixture was concentrated
  5. additionadded EtOH
  6. filtrationfiltered
  7. customThe filtrate was evaporated in vacuo
  8. customthe crude residue was purified over silica gel (60-120 M, 30% EtOAc-Hexane)

出典と根拠

ORDレコード
ord-4b8a3b32071b4f4ba96b0764b952141f
出典データセット
uspto-grants-2013_04
特許番号
US08415383B2

反応ノート

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