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Imidazole → HCID 19603523, 화합물

HRID 1604532
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HRID 1604532 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[OH:9].N1C=CN=C1.[CH:15]([Si:18](Cl)([CH:22]([CH3:24])[CH3:23])[CH:19]([CH3:21])[CH3:20])([CH3:17])[CH3:16]>CN(C)C=O.O>[Cl:8][C:6]1[CH:5]=[CH:4][C:3]([O:9][Si:18]([CH:22]([CH3:24])[CH3:23])([CH:19]([CH3:21])[CH3:20])[CH:15]([CH3:17])[CH3:16])=[C:2]([Cl:1])[CH:7]=1
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참가 물질

6

반응물 3

HCID 795ImidazoleHCID 84492,4-DichlorophenolHCID 139400Triisopropylsilyl chloride

생성물 1

HCID 19603523HCID 19603523, 화합물수율 81.7%

시약·촉매·용매 2

HCID 962Water용매2회HCID 6228Dimethylformamide용매

실험 절차

To a mixture of 2,4-dichlorophenol (3.20 g) and imidazole (2.67 g) in dimethylformamide (30 ml) was added triisopropylsilyl chloride (3.97 g) in water bath under nitrogen atmosphere, and the mixture was stirred for 3 hours under the same condition. The mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with water and brine, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (n-hexane) to give 1,3-dichloro-4-triisopropylsilyloxybenzene (5.12 g).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by silica gel column chromatography (n-hexane)

출처 및 근거

ORD 기록
ord-fb1dfc6ff76946a7bb338a976b7c0d78
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05994368

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