Nitromethane → 1,2-Benzenediol, 4-(2-nitroethenyl)-

HRID 38314

反応式

HRID 38314 の反応式
C([O-])(=O)C.[NH4+].[OH:6][C:7]1[CH:8]=[C:9]([CH:12]=[CH:13][C:14]=1[OH:15])[CH:10]=O.[N+:16]([CH3:19])([O-:18])=[O:17]>>[N+:16]([CH:19]=[CH:10][C:9]1[CH:8]=[C:7]([OH:6])[C:14]([OH:15])=[CH:13][CH:12]=1)([O-:18])=[O:17]

参加物

4

反応物 3

HCID 6375NitromethaneHCID 87683,4-DihydroxybenzaldehydeHCID 517165Ammonium Acetate

生成物 1

HCID 54872581,2-Benzenediol, 4-(2-nitroethenyl)-収率 61%

実験手順

Ammonium acetate (5.6 g, 72.73 mmol, 1.00 equiv) was added to a solution of 3,4-dihydroxybenzaldehyde (10 g, 72.41 mmol, 1.00 equiv) and nitromethane (50 mL). The resulting mixture was heated at reflux for about 16 hours, and then concentrated in vacuo. The resulting residue was then purified by silica gel column chromotagraphy (ethyl acetate/petroleum ether (1:5)) to give the title compound as a yellow oil (8 g, yield=61%).

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux for about 16 hours
  3. concentrationconcentrated in vacuo
  4. customThe resulting residue was then purified by silica gel column chromotagraphy (ethyl acetate/petroleum ether (1:5))

出典と根拠

ORDレコード
ord-948b2595e32c48ddb6b3bc450387cff4
出典データセット
uspto-grants-2013_09
特許番号
US08524733B2

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