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

HRID 1510430노트

반응식

HRID 1510430 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d664394c9fa947bf90b467bb07255144
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08211927B2

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