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Diisobutylaluminumhydride → (7-Bromobenzofuran-5-yl)methanol

HRID 1063841
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HRID 1063841 반응식
C[O:2][C:3]([C:5]1[CH:6]=[C:7]([Br:14])[C:8]2[O:12][CH:11]=[CH:10][C:9]=2[CH:13]=1)=O.[H-].C([Al+]CC(C)C)C(C)C>C1(C)C=CC=CC=1>[OH:2][CH2:3][C:5]1[CH:6]=[C:7]([Br:14])[C:8]2[O:12][CH:11]=[CH:10][C:9]=2[CH:13]=1
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참가 물질

4

반응물 2

HCID 21225700DiisobutylaluminumhydrideHCID 22144801HCID 22144801, 화합물

생성물 1

HCID 22144918(7-Bromobenzofuran-5-yl)methanol수율 82.4%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 0.63 gm (2.46 mmol) 5-methoxycarbonyl-7-bromobenzofuran in 10 mL toluene was cooled to −78° C. When material precipitated, 5 mL dichloromethane were added to effect solution. To this solution were then slowly added 1.5 mL (8.6 mmol) diisobutylaluminum hydride and the reaction mixture was allowed to warm gradually to room temperature. After 10 minutes the reaction was quenched by the addition of methanol followed by 1.5 gm sodium fluoride and 50 mL water and then Rochelle's salt solution. The mixture was diluted with additional dichloromethane and was stirred vigorously for about 1 hour. The phases were separated and the aqueous phase extracted well with ethyl acetate. The organic phases were combined and concentrated under reduced pressure. The residue was crystallized from hexane and dichloromethane to provide 0.46 gm (82%) of the title compound as a white crystalline solid.

후처리

  1. customWhen material precipitated
  2. addition5 mL dichloromethane were added to effect solution
  3. customAfter 10 minutes the reaction was quenched by the addition of methanol
  4. additionThe mixture was diluted with additional dichloromethane
  5. customThe phases were separated
  6. extractionthe aqueous phase extracted well with ethyl acetate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was crystallized from hexane and dichloromethane

출처 및 근거

ORD 기록
ord-340ac47688b94291ac99e50e02c897e9
출처 데이터셋
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06967201B1

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