Hydroxyamine hydrochloride → Methyl 4-(5-(4-(pentyloxy)phenyl)isoxazol-3-yl)benzoate

HRID 1386593노트

반응식

HRID 1386593 반응식
[CH3:1][O:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11](=O)[CH2:12][C:13]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[CH:17][CH:16]=2)=[O:14])=[CH:7][CH:6]=1)=[O:4].Cl.[NH2:29]O>CO.C(OCC)(=O)C>[CH2:22]([O:21][C:18]1[CH:19]=[CH:20][C:15]([C:13]2[O:14][N:29]=[C:11]([C:8]3[CH:9]=[CH:10][C:5]([C:3]([O:2][CH3:1])=[O:4])=[CH:6][CH:7]=3)[CH:12]=2)=[CH:16][CH:17]=1)[CH2:23][CH2:24][CH2:25][CH3:26]

참가 물질

5

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 11405985Methyl 4-[1,3-dioxo-3-[4-(pentyloxy)phenyl]propyl]benzoate

생성물 1

HCID 10737571Methyl 4-(5-(4-(pentyloxy)phenyl)isoxazol-3-yl)benzoate수율 74.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

The solution of 1-(4-Methoxycarbonylphenyl)-3-(4-pentyloxyphenyl)propane-1,3-dione (1.00 g) and hydroxylamine hydrochloride (567 mg) in methanol (10 ml) was refluxed for 10 hours. The reaction mixture was diluted with ethyl acetate (50 ml) and washed with water (50 ml×2), brine (50 ml). The organic layer was dried over magnesium sulfate and the solvents were removed under reduced pressure. The residue was triturated with acetonitrile (10 ml), collected by filtration, and dried under reduced pressure to give Methyl 4-[5-(4-pentyloxyphenyl)isoxazol-3-yl]benzoate (0.74 g).

후처리

  1. washwashed with water (50 ml×2), brine (50 ml)
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. customthe solvents were removed under reduced pressure
  4. customThe residue was triturated with acetonitrile (10 ml)
  5. filtrationcollected by filtration
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-c018834c36c34c2984f15ae90474f41d
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06265536B1

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