Hydroxyamine hydrochloride → Ethyl 5-(4-chlorophenyl)-4-methylisoxazole-3-carboxylate

HRID 1510430ノート

反応式

HRID 1510430 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:18])[CH:9]([CH3:17])[C:10](=O)[C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:4][CH:3]=1.Cl.[NH2:20]O>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:18][N:20]=[C:10]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:9]=2[CH3:17])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 5051380Ethyl 4-(4-chlorophenyl)-3-methyl-2,4-dioxobutanoate

生成物 1

HCID 67121076Ethyl 5-(4-chlorophenyl)-4-methylisoxazole-3-carboxylate収率 3.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The lithium enolate of ethyl 4-(4-chlorophenyl)-3-methyl-2,4-dioxobutanoate (1.5 g, 5.5 mmol) and hydroxylamine hydrochloride (0.46 g, 6.6 mmol) in absolute ethanol (30 mL) were heated to reflux for 17 hours, cooled to room temperature, then cooled to 0° C. for 3 hours. The resulting white crystals were collected and dried under vacuum to obtain ethyl 5-(4-chlorophenyl)-4-methylisoxazole-3-carboxylate (0.55 g, 0.20 mmol).

後処理

  1. temperatureto reflux for 17 hours
  2. temperaturecooled to 0° C. for 3 hours
  3. customThe resulting white crystals were collected
  4. customdried under vacuum

出典と根拠

ORDレコード
ord-d664394c9fa947bf90b467bb07255144
出典データセット
uspto-grants-2012_07
特許番号
US08211927B2

反応ノート

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