Potassium Carbonate → 2,4-Difluoro-benzaldehyde oxime

HRID 497511ノート

反応式

HRID 497511 の反応式
[F:1][C:2]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:3]=1[CH:4]=O.Cl.[OH:12][NH2:13].C([O-])([O-])=O.[K+].[K+]>CCO.CO>[F:1][C:2]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:3]=1[CH:4]=[N:13][OH:12]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 737702,4-DifluorobenzaldehydeHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 533950272,4-Difluoro-benzaldehyde oxime収率 94.6%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol溶媒

実験手順

(Scheme 1, Compound C) To a mixture of 2,4-difluorobenzaldehyde (0.80 g, 5.6 mmol) and hydroxyamine HCl salt (0.43 g, 6.2 mmol) in EtOH (5 mL) was added K2CO3 (0.85 g, 6.2 mmol). The resultant mixture was stirred at rt for 24 hours. The mixture was diluted with MeOH (20 mL). The precipitates were filter off and washed with MeOH. The product from filtrate was purified by recrystalization (EtOAc/Hexanes). This compound was obtained as a white solid (0.84 g, 5.3 mmol, 94% yield). 1H NMR (DMSO-d6) δ 12.98 (br. s, 1H), 8.17 (s, 1H), 7.79 (m, 1H), 7.32 (m, 1H), 7.11 (m, 1H); Analytical HPLC 1.03 min. (95%); Mass Spec.: 158.06 (MH+).

後処理

  1. filtrationThe precipitates were filter off
  2. washwashed with MeOH
  3. customThe product from filtrate was purified by recrystalization (EtOAc/Hexanes)

出典と根拠

ORDレコード
ord-069ed5cc32b84dba804f8537909d11f8
出典データセット
uspto-grants-2005_09
特許番号
US06949574B2

反応ノート

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