Sodium Hydroxide → 3-Methylindan-1-one oxime

HRID 447579

反応式

HRID 447579 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 28186713-Methylindan-1-one oxime

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-4b3ece9ae9484bfd8bffe453d0cc7e8c
出典データセット
uspto-grants-2013_07
特許番号
US08481550B2

関連ノート

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