3-Chlorobenzaldehyde → Benzaldehyde, m-chloro-, oxime, (Z)-

HRID 331813ノート

反応式

HRID 331813 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=O.Cl.[NH2:11][OH:12].C([O-])(=O)C.[Na+]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)/[CH:5]=[N:11]\[OH:12]

参加物

5

反応物 3

HCID 114773-ChlorobenzaldehydeHCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium Acetate

生成物 1

HCID 5372364Benzaldehyde, m-chloro-, oxime, (Z)-収率 98%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of 3-chlorobenzaldehyde (50 g, 355 mmol) and hydroxylamine hydrochloride (38 g, 543 mmol) in ethanol (200 mL) containing sodium acetate (46 g, 558 mmol) was heated under reflux for 3 h. 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 (54 g, 98%) which was obtained as a white solid. Mp: 64-66° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 3 h
  3. customprecipitated
  4. additionthe resulting mixture was then diluted with water
  5. filtrationThe white precipitate was then filtered off
  6. washwashed with water
  7. customdried under high vacuum

出典と根拠

ORDレコード
ord-df067ac24d3645e99b54c30482841de7
出典データセット
uspto-grants-2014_11
特許番号
US08877782B2

反応ノート

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