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

HRID 466994

反応式

HRID 466994 の反応式
[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]

参加物

3

反応物 2

HCID 944Nitric AcidHCID 748423,4-Dimethoxybenzonitrile

生成物 1

HCID 15112884,5-Dimethoxy-2-nitrobenzonitrile収率 98%

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-b7c8968b282341dc9153edda70f07640
出典データセット
uspto-grants-1992_10
特許番号
US05158953

関連ノート

読み込み中…