Hydroxyamine hydrochloride → 2-Fluoro-3-methoxybenzaldehyde oxime

HRID 632922ノート

反応式

HRID 632922 の反応式
C(=O)([O-])O.[Na+].Cl.[NH2:7][OH:8].[F:9][C:10]1[C:17]([O:18][CH3:19])=[CH:16][CH:15]=[CH:14][C:11]=1[CH:12]=O>O.C(O)C>[F:9][C:10]1[C:17]([O:18][CH3:19])=[CH:16][CH:15]=[CH:14][C:11]=1[CH:12]=[N:7][OH:8]

参加物

6

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 37744632-Fluoro-3-methoxybenzaldehyde

生成物 1

HCID 762208362-Fluoro-3-methoxybenzaldehyde oxime収率 85.3%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a stirred solution of sodium hydrogen carbonate (2.73 g, 32.5 mmol) in water (50 mL) was added hydroxylamine hydrochloride (2.30 g, 33.2 mmol) in portions over 30 min. The resultant solution was added to a vigorously stirred suspension of 2-fluoro-3-methoxybenzaldehyde (5.00 g, 32.5 mmol) in ethanol (45 mL) and the reaction mixture stirred at RT for 16 hr. The resultant precipitate was removed by filtration and washed with water (3×100 mL) and then allowed to dry in air to afford 2-fluoro-3-methoxybenzaldehyde oxime (14) (4.69 g, 85%) as a white crystalline solid: m/z 170 (M+H)+ (ES+).

後処理

  1. customThe resultant precipitate was removed by filtration
  2. washwashed with water (3×100 mL)
  3. customto dry in air

出典と根拠

ORDレコード
ord-a1ab1f1263504e928cc902a6c56cfaea
出典データセット
uspto-grants-2016_04
特許番号
US09321773B2

反応ノート

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