Sodium Hydroxide → HCID 178491837, 화합물

HRID 1963006노트

반응식

HRID 1963006 반응식
[F:1][C:2]1[C:9]([O:10][CH3:11])=[CH:8][CH:7]=[C:6]([F:12])[C:3]=1[C:4]#[N:5].Cl.[NH2:14][OH:15].[OH-].[Na+]>CCO>[F:1][C:2]1[C:9]([O:10][CH3:11])=[CH:8][CH:7]=[C:6]([F:12])[C:3]=1[C:4]([NH:14][OH:15])=[NH:5]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 37918322,6-Difluoro-3-methoxybenzonitrile

생성물 1

HCID 178491837HCID 178491837, 화합물수율 43.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 2,6-difluoro-3-methoxybenzonitrile (0.30 g, 1.70 mmol) in EtOH (10 ml) was added hydroxylamine hydrochloride (0.12 g, 1.70 mmol) and NaOH (0.071 g, 1.70 mmol). The resulting reaction mixture was refluxed for 15 h. After the completion of the reaction (TLC monitoring), the mixture was concentrated, added EtOH and filtered. The filtrate was evaporated in vacuo and the crude residue was purified over silica gel (60-120 M, 30% EtOAc-Hexane) to get the desired product (0.15 g, 42%) as a white solid.

후처리

  1. customThe resulting reaction mixture
  2. temperaturewas refluxed for 15 h
  3. customAfter the completion of the reaction (TLC monitoring)
  4. concentrationthe mixture was concentrated
  5. additionadded EtOH
  6. filtrationfiltered
  7. customThe filtrate was evaporated in vacuo
  8. customthe crude residue was purified over silica gel (60-120 M, 30% EtOAc-Hexane)

출처 및 근거

ORD 기록
ord-4b8a3b32071b4f4ba96b0764b952141f
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08415383B2

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