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

HRID 2182735노트

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HRID 2182735 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-d24ac058098d43ec97c3db406218257f
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06897224B2

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