Hypochlorite → Methyl 2,4-dichloro-3-(3-t-butyl-4,5-dihydroisoxazol-5-yl)benzoate

HRID 859098

反応式

HRID 859098 の反応式
Cl[O-].[Na+].[Cl:4][C:5]1[C:14]([CH:15]=[CH2:16])=[C:13]([Cl:17])[CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8].[CH3:18][C:19]([CH3:24])([CH3:23])[CH:20]=[N:21][OH:22].Cl[O-]>ClCCl.O>[Cl:4][C:5]1[C:14]([CH:15]2[O:22][N:21]=[C:20]([C:19]([CH3:24])([CH3:23])[CH3:18])[CH2:16]2)=[C:13]([Cl:17])[CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8]

参加物

7

反応物 4

HCID 61739HypochloriteHCID 136457PivalaldoximeHCID 18769998Methyl 2,4-dichloro-3-ethenylbenzoateHCID 23665760Sodium Hypochlorite

生成物 1

HCID 18770001Methyl 2,4-dichloro-3-(3-t-butyl-4,5-dihydroisoxazol-5-yl)benzoate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

At room temperature, 17 ml of a 12% strength aqueous sodium hypochlorite solution were added dropwise with vigorous stirring to a solution of 2.6 g (10 mmol) of methyl 2,4-dichloro-3-ethenylbenzoate and 1 g (10 mmol) of 2,2-dimethylpropionaldoxime in 100 ml of dichloromethane. Twice, in each case after 2 hours of stirring, a further 0.5 g (5 mmol) of the oxime and 9 ml of the hypochlorite solution were added. The reaction mixture was stirred at room temperature for a further 12 hours and then stirred into 350 ml of water. After extraction with dichloromethane, drying and removal of the solvent, the residue was chromatographed.

後処理

  1. stirringThe reaction mixture was stirred at room temperature for a further 12 hours
  2. extractionAfter extraction with dichloromethane
  3. customdrying
  4. customremoval of the solvent
  5. customthe residue was chromatographed

出典と根拠

ORDレコード
ord-5fa49c6a40804c33a8442e2eb1ec76b4
出典データセット
uspto-grants-2006_12
特許番号
US07151075B2

関連ノート

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