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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → 5,7-Difluoro-4-methyl-3,4-dihydro-2H-chromen-4-ol

HRID 561495
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인쇄 미리보기

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HRID 561495 반응식
[F:1][C:2]1[CH:11]=[C:10]([F:12])[CH:9]=[C:8]2[C:3]=1[C:4](=[O:13])[CH2:5][CH2:6][O:7]2.[CH3:14][Mg]Br.O>C(OCC)C>[F:1][C:2]1[CH:11]=[C:10]([F:12])[CH:9]=[C:8]2[C:3]=1[C:4]([CH3:14])([OH:13])[CH2:5][CH2:6][O:7]2
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참가 물질

5

반응물 3

HCID 962WaterHCID 468354275,7-Difluorochroman-4-oneHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 583921705,7-Difluoro-4-methyl-3,4-dihydro-2H-chromen-4-ol

시약·촉매·용매 1

HCID 3283Diethyl Ether용매3회

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온도
0 °C

실험 절차

2.00 g (10.86 mmol) of the compound from Example 170A were dissolved in 40 ml of diethyl ether at 0° C., and 5.4 ml (16.29 mmol) of a 3N solution of methylmagnesium bromide in diethyl ether were slowly added dropwise. Stirring at 0° C. for 1 h was followed by warming to RT, addition of water and diethyl ether to the reaction solution and separation of the phases. The aqueous phase was extracted with diethyl ether, and the combined organic phases were dried over sodium sulfate and filtered, and the solvents were removed in vacuo. The crude product was purified by flash chromatography on silica gel (mobile phase: dichloromethane). 2.03 g (93% of theory) of the title compound were obtained.

후처리

  1. temperatureby warming to RT
  2. customto the reaction solution and separation of the phases
  3. extractionThe aqueous phase was extracted with diethyl ether
  4. dry with materialthe combined organic phases were dried over sodium sulfate
  5. filtrationfiltered
  6. customthe solvents were removed in vacuo
  7. customThe crude product was purified by flash chromatography on silica gel (mobile phase: dichloromethane)

출처 및 근거

ORD 기록
ord-694613f9486e42caa295f72a8f153267
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08063234B2

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