Water → 3-Nitro-2,6-xylenol

HRID 446330

反応式

HRID 446330 の反応式
[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4]([CH3:11])[C:3]=1N.N([O-])=[O:14].[Na+].O>S(=O)(=O)(O)O>[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4]([CH3:11])[C:3]=1[OH:14]

参加物

5

反応物 3

HCID 962WaterHCID 959453-Nitro-2,6-xylidineHCID 23668193Sodium Nitrite

生成物 1

HCID 814763-Nitro-2,6-xylenol

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

反応条件

温度
0 °C

実験手順

2,6-Dimethyl-3-nitrobenzenamine (10.4 g, 62.6 mmol) was dissolved in 75% sulfuric acid (200 ml). Mixture cooled to 0° C. and treated with a solution of sodium nitrite (4.53 g, 65.7 mmol) in concentrated sulfuric acid (25.0 ml). After the mixture had been stirred for 1 hour at this temperature, water (200 ml) was added and the mixture warmed to 60° C. until the evolution of gas ceased. The mixture was allowed to cool to room temperature and then filtered to afford 2,6-dimethyl-3-nitrophenol. MS m/z=168 (M+H)+. Calc'd for C8H9NO3: 169.18.

後処理

  1. additionwas added
  2. temperaturethe mixture warmed to 60° C. until the evolution of gas
  3. temperatureto cool to room temperature
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-eba43b23bf0c4f6fb897cfbb1b90d637
出典データセット
uspto-grants-2013_07
特許番号
US08476434B2

関連ノート

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