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Epichlorohydrin → HCID 12114671, 화합물

HRID 397598
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인쇄 미리보기

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HRID 397598 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]([C:20]2[CH:25]=[CH:24][C:23]([OH:26])=[C:22](C)[CH:21]=2)[C:10]2[C:19]3[CH2:18][CH2:17][CH2:16][CH2:15][C:14]=3[CH:13]=[CH:12][CH:11]=2)=[CH:5][CH:4]=1.[CH2:28]([CH:30]1[O:32][CH2:31]1)Cl.C([O-])([O-])=O.[K+].[K+]>C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]([C:20]2[CH:21]=[CH:22][C:23]([O:26][CH2:28][CH:30]3[O:32][CH2:31]3)=[CH:24][CH:25]=2)[C:10]2[C:19]3[CH2:18][CH2:17][CH2:16][CH2:15][C:14]=3[CH:13]=[CH:12][CH:11]=2)=[CH:5][CH:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7835EpichlorohydrinHCID 11430Potassium CarbonateHCID 12114667HCID 12114667, 화합물

생성물 1

HCID 12114671HCID 12114671, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
120 °C

실험 절차

A mixture of (4-methoxyphenyl)-(3-methyl-4-hydroxyphenyl)-5,6,7,8-tetrahydronaphth-1-yl-methane (410 mg, 0.001 mol), epichlorohydrin (25 ml) and anhydrous K2CO3 (2.0 gm, 0.014 mol) was refluxed at 120° C. for 6 hrs, K2CO3 was filtered off and the filtrate was concentrated. The residue obtained was dissolved in ethyl acetate and washed with water, dried over sodium sulphate and concentrated to give an oil which was chromatographed over silica gel using hexane:chloroform as the eluent to give the title compound. Yield 388 mg (82.37%).

후처리

  1. filtrationK2CO3 was filtered off
  2. concentrationthe filtrate was concentrated
  3. customThe residue obtained
  4. washwashed with water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated
  7. customto give an oil which
  8. customwas chromatographed over silica gel

출처 및 근거

ORD 기록
ord-ea36be1bcf9d487eab3f3b6cbbd892d7
출처 데이터셋
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06610705B1

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