Water → 1-Methoxy-2-methyl-4-nitrobenzene

HRID 866006

반응식

HRID 866006 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[O:8][CH3:9].F[B-](F)(F)F.[O:15]=[N+:16]=[O:17].O>ClCCl>[CH3:1][C:2]1[CH:7]=[C:6]([N+:16]([O-:17])=[O:15])[CH:5]=[CH:4][C:3]=1[O:8][CH3:9]

참가 물질

5

반응물 3

HCID 962WaterHCID 336372-MethylanisoleHCID 11073463Nitronium tetrafluoroborate

생성물 1

HCID 6435201-Methoxy-2-methyl-4-nitrobenzene

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2-Methylanisole (20 g) in 500 ml dichloromethane chilled in an ice bath is treated with 27.2 g of nitronium tetrafluoroborate and stirred two days. The mixture is poured into water, the layers are separated, and the aqueous phase is washed with dichloromethane. The combined organic layers are dried, filtered, stripped, and chromatographed on silica gel with 9:1 to 8:2 hexane:ethyl acetate to give 2-methyl-4-nitroanisole. NMR (CDCl3): δ2.3 (3H,s), 3.9 (3H,s), 6.9 (1H,d), 8.0 (1H,d), 8.1 (1H,d of d).

후처리

  1. customthe layers are separated
  2. washthe aqueous phase is washed with dichloromethane
  3. customThe combined organic layers are dried
  4. filtrationfiltered
  5. customchromatographed on silica gel with 9:1 to 8:2 hexane

출처 및 근거

ORD 기록
ord-2a846899eb76410098f234781abe39dc
출처 데이터셋
uspto-grants-1996_10
특허 번호
US05569674

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