Potassium Carbonate → 2,4-Difluoro-benzaldehyde oxime

HRID 497511노트

반응식

HRID 497511 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 533950272,4-Difluoro-benzaldehyde oxime수율 94.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 887Methanol용매

실험 절차

(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+).

후처리

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

출처 및 근거

ORD 기록
ord-069ed5cc32b84dba804f8537909d11f8
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06949574B2

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