Cyclohexyl phenyl ketone → Cyclohexyl-phenyl-methanone oxime

HRID 271838

反応式

HRID 271838 の反応式
Cl.[NH2:2][OH:3].C([O-])(=O)C.[Na+].[CH:9]1([C:15]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=O)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1>CO>[CH:9]1([C:15]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[N:2][OH:3])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1

参加物

5

反応物 3

HCID 12837Cyclohexyl phenyl ketoneHCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium Acetate

生成物 1

HCID 346900Cyclohexyl-phenyl-methanone oxime

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Hydroxylamine hydrochloride (0.48 g, 6.7 mMol) and sodium acetate (1.4 g, 10.2 mMol) were added to a round bottom flask containing cyclohexyl-phenyl-methanone Compound 18a (0.97 g, 5.1 mMol) in MeOH (30 mL) at r.t. The mixture was stirred at r.t. for 15 hrs. The solvent was removed in vacuo and the residue was extracted with CH2Cl2. The organic layer was sequentially washed with a saturated solution of NaHCO3, then brine. The organic layer was dried over Na2SO4, decanted and the solvent removed in vacuo to provide cyclohexyl-phenyl-methanone oxime Compound 18b (1.0 g) as a white solid, which was used in the next step without purification. MS m/z 204 (MH+).

後処理

  1. customThe solvent was removed in vacuo
  2. extractionthe residue was extracted with CH2Cl2
  3. washThe organic layer was sequentially washed with a saturated solution of NaHCO3
  4. dry with materialThe organic layer was dried over Na2SO4
  5. customdecanted
  6. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-83d6825bf7914461b78e20bc77d4d6a9
出典データセット
uspto-grants-2008_11
特許番号
US07452997B2

関連ノート

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