Sodium Hydroxide → (E)-N-[(3-Fluorophenyl)methylidene]hydroxylamine

HRID 331799

반응식

HRID 331799 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=O.Cl.[NH2:11][OH:12].[OH-].[Na+]>C(O)C.O>[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)/[CH:5]=[N:11]\[OH:12]

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 680093-FluorobenzaldehydeHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 5582750(E)-N-[(3-Fluorophenyl)methylidene]hydroxylamine수율 93.2%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

To a suspension of 3-fluorobenzaldehyde (6.75 g, 54 mmol) and hydroxylamine hydrochloride (4.16 g, 60 mmol) in ethanol (4.3 mL) and water (13 mL) was added ice (25 g). Then a solution of sodium hydroxide (5.5 g, 138 mmol) in water (6.5 mL) was added dropwise within a 10 min period (temperature rises from −8° C. to +7° C.) whereupon most of the solid dissolves. 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 (7.0 g, 93%) which was obtained as a white solid. MS m/e (EI): 139.1 [M].

후처리

  1. dissolutiondissolves
  2. customprecipitated
  3. additionthe resulting mixture was then diluted with water
  4. filtrationThe white precipitate was then filtered off
  5. washwashed with water
  6. customdried under high vacuum

출처 및 근거

ORD 기록
ord-a10c27878a3246db9d9dbdaef9d4e59c
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877782B2

연결된 노트

불러오는 중…