反応 #684448

反応方程式

3-hydroxy biphenyl

dimethyl sulphate

dimethyl sulphate

→

3-methoxy biphenyl

溶媒

water

potassium hydroxide

potassium hydroxide

water

反応条件

後処理

1. 1
   workup.WAITThe mixture is again kept at 75° for 1 hour
2. 2
   温度After cooling
3. 3
   その他the oily layer is separated
4. 4
   洗浄Washing
5. 5
   抽出Extraction
6. 6
   乾燥dried over anhydrous sodium sulphate
7. 7
   濃縮concentrated

実験手順

102 g of 3-hydroxy biphenyl are dissolved in a solution of 67.8 g of potassium hydroxide in 650 cc of water. 86.6 cc of dimethyl sulphate are added dropwise within 30 minutes while stirring, whereby the reaction mixture warms itself. The reaction mixture is then kept at 75° for a further 15 minutes. After 1 hour a further 33.6 g of potassium hydroxide in 45 cc of water are added dropwise, and subsequently 37.8 g of dimethyl sulphate are added dropwise at 65° within 15 minutes. The mixture is again kept at 75° for 1 hour. After cooling, the oily layer is separated and taken up in methylene chloride. Washing is effected once with 2 N sodium hydroxide and once with water. Extraction is again effected twice with methylene chloride. The organic phases are combined, dried over anhydrous sodium sulphate and concentrated. 3-methoxy biphenyl is obtained and is used for the next reaction step without purification.

出典