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Methyl iodide → HCID 22995024, 화합물

HRID 1168042
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HRID 1168042 반응식
[Br:1][C:2]1[C:3]([OH:16])=[CH:4][C:5]2[C:6]3([CH3:15])[CH2:13][CH2:12][C:9]([CH3:14])([C:10]=2[CH:11]=1)[CH2:8][CH2:7]3.[C:17](=O)([O-])[O-].[K+].[K+].IC>CC(C)=O>[Br:1][C:2]1[C:3]([O:16][CH3:17])=[CH:4][C:5]2[C:6]3([CH3:15])[CH2:13][CH2:12][C:9]([CH3:14])([CH2:8][CH2:7]3)[C:10]=2[CH:11]=1
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 22995025HCID 22995025, 화합물2회

생성물 1

HCID 22995024HCID 22995024, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

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온도
25 °C

실험 절차

To a solution of 5-bromo-1,8-dimethyl-tricyclo[6.2.2.02,7]dodeca-2(7),3,5-trien-4-ol (Compound 3, 0.825 g, 2.94 mmol) in 10 mL of anhydrous acetone was added potassium carbonate (0.128 g, 8.82 mmol) and iodomethane (0.1 mL, 8.82 mmol). The reaction mixture was stirred at 25° C. for 12 hours and filtered. The filtrate was concentrated, and then it was diluted with ether and washed with water and brine. The organic layer was dried over Na2SO4, and filtered, and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using ethyl acetate:hexane (5:95) to yield the title compound as a white solid.

후처리

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated
  3. additionit was diluted with ether
  4. washwashed with water and brine
  5. dry with materialThe organic layer was dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-70bdb253e41b439a89daa16f987d37ab
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06620963B1

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