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Pyridine → 1-(Bromomethyl)-2-methoxy-3-nitrobenzene

HRID 618244
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HRID 618244 반응식
[CH3:1][O:2][C:3]1[C:8]([N+:9]([O-:11])=[O:10])=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:12]O.N1C=CC=CC=1.P(Br)(Br)[Br:21]>ClCCl>[Br:21][CH2:12][C:4]1[CH:5]=[CH:6][CH:7]=[C:8]([N+:9]([O-:11])=[O:10])[C:3]=1[O:2][CH3:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 24614Phosphorus tribromideHCID 18789679(2-Methoxy-3-nitrophenyl)methanol

생성물 1

HCID 186220771-(Bromomethyl)-2-methoxy-3-nitrobenzene

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 14.7 g of (2-methoxy-3-nitro-phenyl)-methanol dissolved in 140 ml of dichloromethane and 5.5 ml of pyridine was cooled in an ice bath and slowly added 6.48 ml of phosphorus tribromide. After 45 minutes at 5° C., the reaction mixture was diluted with dichloromethane, washed with water, dried, and evaporated to dryness. The residue was purified by flash chromatography on silica gel eluting with ethyl acetate/hexane (5:95) giving 7.3 g of 1-bromomethyl-2-methoxy-3-nitrobenzene as a yellow solid. ##STR137##

후처리

  1. washwashed with water
  2. customdried
  3. customevaporated to dryness
  4. customThe residue was purified by flash chromatography on silica gel eluting with ethyl acetate/hexane (5:95)

출처 및 근거

ORD 기록
ord-8c50ffb64fc943a28a3b698344fe465e
출처 데이터셋
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05952362

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