Sodium Hydroxide → (E)-N-[(3-Fluorophenyl)methylidene]hydroxylamine

HRID 548847

反応式

HRID 548847 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=O.Cl.[NH2:11][OH:12].[OH-].[Na+]>C(O)C.O>[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)/[CH:5]=[N:11]\[OH:12]

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 680093-FluorobenzaldehydeHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 5582750(E)-N-[(3-Fluorophenyl)methylidene]hydroxylamine収率 93.2%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

To a suspension of 3-fluorobenzaldehyde (6.75 g, 54 mmol) and hydroxylamine hydrochloride (4.16 g, 60 mmol) in ethanol (4.3 mL) and water (13 mL) was added ice (25 g). Then a solution of sodium hydroxide (5.5 g, 138 mmol) in water (6.5 mL) was added dropwise within a 10 min period (temperature rises from −8° C. to +7° C.) whereupon most of the solid dissolves. After 30 min stirring at room temperature a white solid precipitated and the resulting mixture was then diluted with water and acidified with HCl (4 N). The white precipitate was then filtered off, washed with water and dried under high vacuum to afford the title compound (7.0 g, 93%) which was obtained as a white solid. MS m/e (EI): 139.1 [M].

後処理

  1. dissolutiondissolves
  2. customprecipitated
  3. additionthe resulting mixture was then diluted with water
  4. filtrationThe white precipitate was then filtered off
  5. washwashed with water
  6. customdried under high vacuum

出典と根拠

ORDレコード
ord-68016671d49d4764a70958adc2caf11a
出典データセット
uspto-grants-2011_05
特許番号
US07943619B2

関連ノート

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