Hydroxyamine hydrochloride → 2-Fluoro-3-methoxybenzaldehyde oxime

HRID 632922

반응식

HRID 632922 반응식
C(=O)([O-])O.[Na+].Cl.[NH2:7][OH:8].[F:9][C:10]1[C:17]([O:18][CH3:19])=[CH:16][CH:15]=[CH:14][C:11]=1[CH:12]=O>O.C(O)C>[F:9][C:10]1[C:17]([O:18][CH3:19])=[CH:16][CH:15]=[CH:14][C:11]=1[CH:12]=[N:7][OH:8]

참가 물질

6

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 37744632-Fluoro-3-methoxybenzaldehyde

생성물 1

HCID 762208362-Fluoro-3-methoxybenzaldehyde oxime수율 85.3%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a stirred solution of sodium hydrogen carbonate (2.73 g, 32.5 mmol) in water (50 mL) was added hydroxylamine hydrochloride (2.30 g, 33.2 mmol) in portions over 30 min. The resultant solution was added to a vigorously stirred suspension of 2-fluoro-3-methoxybenzaldehyde (5.00 g, 32.5 mmol) in ethanol (45 mL) and the reaction mixture stirred at RT for 16 hr. The resultant precipitate was removed by filtration and washed with water (3×100 mL) and then allowed to dry in air to afford 2-fluoro-3-methoxybenzaldehyde oxime (14) (4.69 g, 85%) as a white crystalline solid: m/z 170 (M+H)+ (ES+).

후처리

  1. customThe resultant precipitate was removed by filtration
  2. washwashed with water (3×100 mL)
  3. customto dry in air

출처 및 근거

ORD 기록
ord-a1ab1f1263504e928cc902a6c56cfaea
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321773B2

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