反応式
[CH3:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[C:6]([CH3:8])[CH:7]=1.[N:10]([O-])=[O:11].[Na+]>C(O)C.O>[CH3:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[C:6]([CH3:8])[C:7]=1[N:10]=[O:11]参加物
5
反応条件
- 温度
- 0 °C
実験手順
750 ml of concentrated HClare added to a solution of 3,5-dimethyl phenol (80.6 g) in 750 ml of 95% ethyl alcohol. The mixture is cooled to 0° C. in an ice/methanol bath. While maintaining the temperature of the reaction mixture below 5° C. a solution of NaNO2 (69.0 g) in 150 ml of H2O is added dropwise to the reaction mixture. The mixture is stirred at 0° C. for more than an hour and then poured into 9 liters of water. The aqueous mixture is filtered to give a yellow solid which is recrystallized from hot methanol and filtered to give 71.45 grams of a yellow solid, M.P. 180°-181° C. (dec).
後処理
- additionis added dropwise to the reaction mixture
- filtrationThe aqueous mixture is filtered
- customto give a yellow solid which
- customis recrystallized from hot methanol
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-8747f9542fbf467f9dfa62465296144d
- 出典データセット
- uspto-grants-1986_01
- 特許番号
- US04564640
関連ノート
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