Hydroxyamine hydrochloride → Ethyl 5-(4-(trifluoromethyl)phenyl)isoxazole-3-carboxylate

HRID 1510436

반응식

HRID 1510436 반응식
O=[C:2]([CH2:8][C:9](=[O:20])[C:10]1[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][CH:11]=1)[C:3]([O:5][CH2:6][CH3:7])=[O:4].Cl.[NH2:22]O>C(O)C>[F:17][C:16]([F:19])([F:18])[C:13]1[CH:14]=[CH:15][C:10]([C:9]2[O:20][N:22]=[C:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])[CH:8]=2)=[CH:11][CH:12]=1

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 611940Ethyl 2,4-dioxo-4-[4-(trifluoromethyl)phenyl]butanoate

생성물 1

HCID 22064085Ethyl 5-(4-(trifluoromethyl)phenyl)isoxazole-3-carboxylate수율 65.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of ethyl 2,4-dioxo-4-(4-(trifluoromethyl)phenyl)butanoate (6.89 g, 23.9 mmol) and hydroxylamine hydrochloride (2.0 g, 28.7 mmol) in ethanol (120 mL) was stirred at reflux overnight. The volatiles were removed in vacuo, and the residue purified by silica gel chromatography, eluting with dichloromethane to obtain the title compound (4.5 g, 15.6 mmol).

후처리

  1. temperatureat reflux overnight
  2. customThe volatiles were removed in vacuo
  3. customthe residue purified by silica gel chromatography
  4. washeluting with dichloromethane

출처 및 근거

ORD 기록
ord-855b5b9f7a724f8399e71d0c897e83c5
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08211927B2

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