Hydrochloric Acid → Benzaldehyde, 2-fluoro-, oxime

HRID 83191ノート

反応式

HRID 83191 の反応式
[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=O.Cl.[NH2:11][OH:12].[OH-].[Na+].Cl>C(O)C.O>[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[N:11][OH:12]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 67970o-FluorobenzaldehydeHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 587025Benzaldehyde, 2-fluoro-, oxime収率 97%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a suspension of 2-fluorobenzaldehyde (63.3 g, 495 mmol) and hydroxylamine hydrochloride (38.2 g, 544 mmol) in ethanol (36 mL) and water (69 mL) was added ice (205 g). Then an aqueous solution of sodium hydroxide (32%, 115 mL, 1.24 mol) was added dropwise within a 10 min period (temperature rises from −8° C. to +7° C.) whereupon most of the solid dissolves. After 1 h stirring at room temperature the resulting mixture was then acidified with HCl (5 N). The mixture was then extracted with dichloromethane to afford the title compound (66.8 g, 97%) which was obtained as a light yellow solid. MS m/e (EI): 139.0 [M].

後処理

  1. dissolutiondissolves
  2. extractionThe mixture was then extracted with dichloromethane

出典と根拠

ORDレコード
ord-796b51fae67044e4b73bce12226ac914
出典データセット
uspto-grants-2014_09
特許番号
US08846719B2

反応ノート

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