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Water → 4-Methoxyxanthone

HRID 730066
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인쇄 미리보기

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HRID 730066 반응식
[CH3:1][O:2][C:3]1[CH:18]=[CH:17][CH:16]=[CH:15][C:4]=1[O:5][C:6]1[CH:14]=[CH:13][CH:12]=[CH:11][C:7]=1[C:8]([OH:10])=O.FC(F)(F)C(OC(=O)C(F)(F)F)=O.B(F)(F)F.CCOCC.O>C(Cl)Cl>[CH3:1][O:2][C:3]1[C:4]2[O:5][C:6]3[C:7](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:8](=[O:10])[C:15]=2[CH:16]=[CH:17][CH:18]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 8000Boron trifluoride etherateHCID 9845Trifluoroacetic anhydrideHCID 5786892-(2-Methoxyphenoxy)benzoic acid

생성물 1

HCID 3002414-Methoxyxanthone수율 79.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

To a suspension of 2-(2-methoxy-phenoxy)-benzoic acid (16.8 g, 68.8 mmol) in methylene chloride (100 mL) at 0° C. was added dropwise trifluoroacetic anhydride (12.7 mL, 89.4 mmol), and the reaction was stirred for 30 min at 0° C. At that time, boron trifluoride diethyl etherate (1.29 mL, 10.3 mmol) was added dropwise. The reaction was stirred overnight at rt, poured into H2O, and washed with brine. The organic phase was dried over MgSO4, filtered, and concentrated to give 12.4 g (54.8 mmol) of Compound 2a.

후처리

  1. stirringThe reaction was stirred overnight at rt
  2. washwashed with brine
  3. dry with materialThe organic phase was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-24cbce89319a47ac8d523e3c9b2eee61
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07582650B2

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