Hydroxyamine hydrochloride → Methyl 5-(3-bromophenyl)isoxazole-3-carboxylate

HRID 1375654노트

반응식

HRID 1375654 반응식
[CH3:1][O:2][C:3](=[O:16])[C:4](=O)[CH2:5][C:6](=[O:14])[C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([Br:13])[CH:8]=1.Cl.[NH2:18]O>CO>[CH3:1][O:2][C:3]([C:4]1[CH:5]=[C:6]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([Br:13])[CH:8]=2)[O:14][N:18]=1)=[O:16]

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 17024761Methyl 4-(3-bromophenyl)-2,4-dioxobutanoate

생성물 1

HCID 53393795Methyl 5-(3-bromophenyl)isoxazole-3-carboxylate수율 87.4%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a suspension of 2,4-dioxo-4-(3-bromophenyl)-butyric acid methyl ester (10.3 g, 36.1 mmol) in anhydrous MeOH (100 mL) was added hydroxylamine hydrochloride (3.8 g, 54.2 mmol). The mixture was then refluxed for 90 min. The reaction mixture was then cooled to room temperature, and ice/water mixture (200 mL) was added. The mixture was stirred for 20 minutes, filtered through a Buchner funnel and washed with cold water. The light yellow solid was dried in vacuum oven to provide the title compound (8.9 g, 87% yield).

후처리

  1. temperatureThe mixture was then refluxed for 90 min
  2. filtrationfiltered through a Buchner funnel
  3. washwashed with cold water
  4. customThe light yellow solid was dried in vacuum oven

출처 및 근거

ORD 기록
ord-d459cf83cfac40b18a64af6c1b0c1e6c
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07169797B2

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