Boron tribromide → Benzaldehyde, 2,3-dihydroxy-4-nitro-

HRID 2055017노트

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HRID 2055017 반응식
[OH:1][C:2]1[C:9]([O:10]C)=[C:8]([N+:12]([O-:14])=[O:13])[CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].B(Br)(Br)Br>ClCCl>[OH:1][C:2]1[C:9]([OH:10])=[C:8]([N+:12]([O-:14])=[O:13])[CH:7]=[CH:6][C:3]=1[CH:4]=[O:5]

참가 물질

4

반응물 2

HCID 25134Boron tribromideHCID 149774472-Hydroxy-3-methoxy-4-nitrobenzaldehyde

생성물 1

HCID 10442360Benzaldehyde, 2,3-dihydroxy-4-nitro-수율 95.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

17.2 g of 2-hydroxy-3-methoxy-4-nitrobenzaldehyde (J. Het. Chem. 33, (1996), 1171) in 350 ml of dichloromethane is slowly mixed at 0° C. with 175 ml of boron tribromide solution (1 M in dichloromethane), and it is stirred for another 4 hours. The batch is added to ice water, the organic phase is separated, and the aqueous phase is extracted with dichloromethane. The combined organic phases are washed with water, and the solvent is removed in a vacuum. 15.2 g of 2,3-dihydroxy-4-nitrobenzaldehyde is obtained as a red solid, flash point 122-126° C.

후처리

  1. customthe organic phase is separated
  2. extractionthe aqueous phase is extracted with dichloromethane
  3. washThe combined organic phases are washed with water
  4. customthe solvent is removed in a vacuum

출처 및 근거

ORD 기록
ord-531a81c9364047809724090e922097bd
출처 데이터셋
uspto-grants-2008_02
특허 번호
US07329753B2

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