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Boron tribromide → HCID 18329463, 화합물

HRID 1250088
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HRID 1250088 반응식
B(Br)(Br)Br.[CH:5]([C:8]1[C:16]([O:17]C)=[CH:15][CH:14]=[CH:13][C:9]=1[C:10]([OH:12])=[O:11])([CH3:7])[CH3:6]>ClCCl>[OH:17][C:16]1[C:8]([CH:5]([CH3:7])[CH3:6])=[C:9]([CH:13]=[CH:14][CH:15]=1)[C:10]([OH:12])=[O:11]
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참가 물질

4

반응물 2

HCID 25134Boron tribromideHCID 18329461HCID 18329461, 화합물

생성물 1

HCID 18329463HCID 18329463, 화합물수율 97.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

A solution of 1M boron tribromide in dichloromethane (15 mL, 15 mmol) was added dropwise to a solution of 2-isopropyl-3-methoxybenzoic acid in dichloromethane. After stirring for 2 hours, the reaction mixture was cooled to 0° C., quenched with water, and the layers were separated. The aqueous layer was extracted with dichloromethane. The combined organic extracts were dried over anhydrous sodium sulfate and concentrated in vacuo. Purification of the residue by silica gel flash chromatography, eluting with dichloromethane/methanol and 1% acetic acid, gave 3-hydroxy-2-isopropylbenzoic acid as a white crystalline solid (1.32 g, 97.5%).

후처리

  1. customquenched with water
  2. customthe layers were separated
  3. extractionThe aqueous layer was extracted with dichloromethane
  4. dry with materialThe combined organic extracts were dried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customPurification of the residue by silica gel flash chromatography
  7. washeluting with dichloromethane/methanol and 1% acetic acid

출처 및 근거

ORD 기록
ord-9cd83d8bc03c4059bce9f84d285a781e
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06335459B1

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