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4-Methylbenzaldehyde → 3-(3-Chlorophenyl)-alpha-(4-methylphenyl)-2,1-benzisoxazole-5-methanol

HRID 1441466
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인쇄 미리보기

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HRID 1441466 반응식
[Li]CCCC.CCCCCC.Br[C:13]1[CH:14]=[CH:15][C:16]2[C:17]([CH:28]=1)=[C:18]([C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([Cl:27])[CH:22]=1)[O:19][N:20]=2.[CH3:29][C:30]1[CH:37]=[CH:36][C:33]([CH:34]=[O:35])=[CH:32][CH:31]=1>C1COCC1>[Cl:27][C:23]1[CH:22]=[C:21]([C:18]2[O:19][N:20]=[C:16]3[CH:15]=[CH:14][C:13]([CH:34]([C:33]4[CH:36]=[CH:37][C:30]([CH3:29])=[CH:31][CH:32]=4)[OH:35])=[CH:28][C:17]=23)[CH:26]=[CH:25][CH:24]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 77254-MethylbenzaldehydeHCID 8058HexaneHCID 120166705-Bromo-3-(3-chlorophenyl)-2,1-benzisoxazoleHCID 178418339Butyllithium

생성물 1

HCID 179761013-(3-Chlorophenyl)-alpha-(4-methylphenyl)-2,1-benzisoxazole-5-methanol수율 38.3%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

반응 조건

온도
-70 °C

실험 절차

nBuLi 1.6 M in hexane (0.112 mol) was added dropwise at −70° C. under N2 flow to a mixture of 5-bromo-3-(3-chlorophenyl)-2,1-benzisoxazole (0.097 mol) in THF (300 ml). The mixture was stirred at −70° C. for 15 min. A mixture of 4-methyl-benzaldehyde (0.112 mol) in THF (100 ml) was added dropwise. The mixture was stirred at −70° C. for 30 min, then hydrolized and extracted with EtOAc. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated till dryness. The residue was purified by column chromatography over silica gel (20-45 μm) (eluent: DCM(EtOAc 96/4). The pure fractions were collected and the solvent was evaporated, yielding 13 g (38.3%) of 3-(3-chlorophenyl)-α-(4-methylphenyl)-2,1-benzisoxazole-5-methanol (intermediate 18).

후처리

  1. additionwas added dropwise
  2. stirringThe mixture was stirred at −70° C. for 30 min
  3. extractionhydrolized and extracted with EtOAc
  4. customThe organic layer was separated
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customthe solvent was evaporated till dryness
  8. customThe residue was purified by column chromatography over silica gel (20-45 μm) (eluent
  9. customThe pure fractions were collected
  10. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-7e9957d78fd440c29802b802707c051c
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07655654B2

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