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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → HCID 22090626, 화합물

HRID 1993718
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HRID 1993718 반응식
B(Br)(Br)Br.C[O:6][C:7]1[C:15]2[C:11](=[CH:12][O:13][N:14]=2)[CH:10]=[CH:9][CH:8]=1.O.C(=O)([O-])[O-].[Na+].[Na+]>ClCCl>[N:14]1[O:13][CH:12]=[C:11]2[CH:10]=[CH:9][CH:8]=[C:7]([OH:6])[C:15]=12
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참가 물질

6

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 25134Boron tribromideHCID 118296117-Methoxy-2,1-benzisoxazole

생성물 1

HCID 22090626HCID 22090626, 화합물수율 10%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
-78 °C

실험 절차

18.5 ml of a 1M solution of boron tribromide in dichloromethane are added to a solution of 1.38 g (9.25 mM) of 7-methoxy-2,1-benzisoxazole in 50 ml of dichloromethane cooled to −78° C., and the mixture is then stirred at ambient temperature overnight. The reaction medium is poured into water and the mixture is brought to pH=7-8 by adding a solution of sodium carbonate, and then extracted with dichloromethane. The organic phase is dried over magnesium sulfate and concentrated under vacuum. The crude product obtained is purified by silica gel chromatography, elution being carried out with a methylcyclohexane/ethyl acetate mixture (gradient of 100/0 to 50/50; v/v). The expected product is obtained in the form of a yellow solid with a yield of 10%.

후처리

  1. extractionextracted with dichloromethane
  2. dry with materialThe organic phase is dried over magnesium sulfate
  3. concentrationconcentrated under vacuum
  4. customThe crude product obtained
  5. customis purified by silica gel chromatography, elution

출처 및 근거

ORD 기록
ord-579ced030d5344a1ab70608b0c3082f3
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07652032B2

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