Sodium Hydroxide → 3-Methylindan-1-one oxime

HRID 447579

반응식

HRID 447579 반응식
[CH3:1][CH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=O)[CH2:3]1.Cl.[NH2:13][OH:14].[OH-].[Na+]>CO.O>[CH3:1][CH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[N:13][OH:14])[CH2:3]1

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 2595603-Methyl-indan-1-oneHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 28186713-Methylindan-1-one oxime

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

To a solution of 3-methylindan-1-one (221 mg, 1.51 mmol) and hydroxylamine hydrochloride (295 mg, 4.25 mmol) in MeOH (4.00 mL) was added a solution of NaOH (200 mg, 5.00 mmol) in H2O (2.00 mL) and the mixture was stirred at 80° C. for 2 h. The cooled reaction was concentrated in vacuo to remove most of the MeOH, and the residue was partitioned between DCM and H2O. The organic layer was concentrated in vacuo to afford the title compound as a waxy solid (232 mg, 95%). LC/MS: Rt=1.51 min, ES+ 162 (AA standard).

후처리

  1. customThe cooled reaction
  2. concentrationwas concentrated in vacuo
  3. customto remove most of the MeOH
  4. customthe residue was partitioned between DCM and H2O
  5. concentrationThe organic layer was concentrated in vacuo

출처 및 근거

ORD 기록
ord-4b3ece9ae9484bfd8bffe453d0cc7e8c
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481550B2

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