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Water → Ethyl 5,5-diphenyl-2-isoxazoline-3-carboxylate

HRID 439736
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HRID 439736 반응식
[C:1]1([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH2:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.Cl[C:23](=[N:29][OH:30])[C:24]([O:26][CH2:27][CH3:28])=[O:25].O>CCOCC>[C:1]1([C:7]2([C:9]3[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=3)[O:30][N:29]=[C:23]([C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 107401,1-DiphenylethyleneHCID 6816376Ethyl chloro(hydroximino)acetate

생성물 1

HCID 6451155Ethyl 5,5-diphenyl-2-isoxazoline-3-carboxylate

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

13.52 g (0.075 mol) of 1,1-diphenylethene and 5.06 g (0.05 mol) of triethylamine are dissolved in 200 ml of ether at 0° C., and 7.58 g (0.05 mol) of ethyl 2-chloro-2-hydroximinoacetate, dissolved in 100 ml of ether, are subsequently added dropwise in the course of approximately two hours. After stirring has been continued for one hour at room temperature, 100 ml of H2O are added, and the mixture is subsequently extracted using ether. After drying over a MgSO4, the ether is distilled off and the residue is purified over a silica gel column (eluent: n-heptane:ethyl acetate=8:2). In this way, 12.7 g (86% of theory) of product of melting point 78° to 81° C. are obtained.

후처리

  1. additionare subsequently added dropwise in the course of approximately two hours
  2. extractionthe mixture is subsequently extracted
  3. dry with materialAfter drying over a MgSO4
  4. distillationthe ether is distilled off
  5. customthe residue is purified over a silica gel column (eluent: n-heptane:ethyl acetate=8:2)
  6. customIn this way, 12.7 g (86% of theory) of product of melting point 78° to 81° C. are obtained

출처 및 근거

ORD 기록
ord-6e5d0458f33146dc89aa9bbcaaec6c49
출처 데이터셋
uspto-grants-1996_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05516750

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