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Water → HCID 22398226, 화합물

HRID 1070887
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HRID 1070887 반응식
[CH3:1][C:2]1[C:3]([OH:16])=[CH:4][C:5]2[C:6]([CH3:15])([CH3:14])[CH2:7][CH2:8][C:9]([CH3:13])([CH3:12])[C:10]=2[CH:11]=1.[Br:17]Br.O>C(O)(=O)C>[Br:17][C:4]1[C:5]2[C:6]([CH3:15])([CH3:14])[CH2:7][CH2:8][C:9]([CH3:12])([CH3:13])[C:10]=2[CH:11]=[C:2]([CH3:1])[C:3]=1[OH:16]
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참가 물질

5

반응물 3

HCID 962WaterHCID 24408BromineHCID 2266903,5,5,8,8-Pentamethyl-5,6,7,8-tetrahydro2-naphthol

생성물 1

HCID 22398226HCID 22398226, 화합물수율 92.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

In 500 mL roundbottom flask, 3,5,5,8,8-pentamethyl-5,6,7,8-tetrahydro-2-naphthalenol (10.2 g, 46.72 mmol) was dissolved in 100 mL Acetic Acid. To this solution Bromine (8.2 g, 51.39 mmol) was added. The reaction was stirred at room temperature for 20 minutes. The reaction mixture was poured into water and extracted with ethyl acetate. The separated organic layer was washed with brine, dried over magnesium sulfate and concentrated. The crude product was purified by silica gel chromatography eluted with hexane to yield 1-Bromo-3,5,5,8,8-pentamethyl-5,6,7,8-tetrahydro-2-naphthalenol (12.8 g, 92% yield).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe separated organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe crude product was purified by silica gel chromatography
  6. washeluted with hexane

출처 및 근거

ORD 기록
ord-da2f84a0de6848c3ab705820fd245ada
출처 데이터셋
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06903132B2

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