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Triethylamine → HCID 12894082, 화합물

HRID 1279393
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HRID 1279393 반응식
[CH3:1][O:2][CH:3]1[O:8][CH2:7][C:6](=[O:9])[CH:5]=[CH:4]1.[Br:10]Br.C(N(CC)CC)C>C(Cl)Cl.C1(C)C=CC=CC=1>[Br:10][C:5]1[C:6](=[O:9])[CH2:7][O:8][CH:3]([O:2][CH3:1])[CH:4]=1
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참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 24408BromineHCID 130117856-methoxy-3,6-dihydro-2H-pyran-3-one

생성물 1

HCID 12894082HCID 12894082, 화합물수율 82.1%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 6-methoxy-2H-pyran-3(6H)-one 12.8 (0.1 mole) in 40 ml CH2Cl2 at 0° C. was added 16.0 g (0.1 mole) of bromine in 10 ml of CH2Cl2. Then 14 ml of triethylamine was added dropwise at 0° C. and the reaction was allowed to warm to room temperature and stir for two hours. The reaction was then diluted with 200 ml of toluene. After filtration, the organic solution was then washed with 5% NaHCO3 and brine, dried with Na2SO4, filtered and concentrated to yield the crude product as light brown solid. Recrystallisation from ethyl acetate afforded the title compound (17 g 82%) as a white crystalline solid.

후처리

  1. filtrationAfter filtration
  2. washthe organic solution was then washed with 5% NaHCO3 and brine
  3. dry with materialdried with Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto yield the crude product as light brown solid
  7. customRecrystallisation from ethyl acetate

출처 및 근거

ORD 기록
ord-b73a8c6d6ae043fc9e4c28f1c649e9b0
출처 데이터셋
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06448273B1

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