Nitric Acid → 4,5-Dimethoxy-2-nitrobenzonitrile

HRID 466994

반응식

HRID 466994 반응식
[N+:1]([O-:4])(O)=[O:2].[CH3:5][O:6][C:7]1[CH:8]=[C:9]([CH:12]=[CH:13][C:14]=1[O:15][CH3:16])[C:10]#[N:11]>>[N+:1]([C:12]1[CH:13]=[C:14]([O:15][CH3:16])[C:7]([O:6][CH3:5])=[CH:8][C:9]=1[C:10]#[N:11])([O-:4])=[O:2]

참가 물질

3

반응물 2

HCID 944Nitric AcidHCID 748423,4-Dimethoxybenzonitrile

생성물 1

HCID 15112884,5-Dimethoxy-2-nitrobenzonitrile수율 98%

실험 절차

To a nitric acid (40 mL) in ice bath was added 3,4-dimethoxybenzonitrile (5.0 g, 30.6 mmol) and was allowed to stir for 2 hours. Then the solution was gradually returned to room temperature. To this solution was added ice (200 mL) to get light yellow precipitate which was then collected by filtration to give 6.25 g (98%) of 2-nitro-4,5-dimethoxybenzonitrile. 1H NMR (100 MHz, DMSO-d6): δ3.69 (s, 3H, CH3), 3.90 (s, 3H, CH3), 7.53 (s, 1H, Ar--H), 7.75 (s, 1H, Ar--H). ms: m/z 208 (M+), 192 (M+ -16), 178 (M+ -30), 162 (M+ -46).

후처리

  1. customwas gradually returned to room temperature
  2. customto get light yellow precipitate which
  3. filtrationwas then collected by filtration

출처 및 근거

ORD 기록
ord-b7c8968b282341dc9153edda70f07640
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05158953

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