反応 #833531

反応方程式

1-chloromethyl-2-methyl-2-propanol

sodium methacrylate

phenothiazine

→

2-hydroxy-2,2-dimethylethyl methacrylate

溶媒

hexane

butyronitrile

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度to reflux under nitrogen in a three-necked round bottomed flask
3. 3
   その他equipped with a condenser and a mechanical stirrer
4. 4
   ろ過filtered through celite
5. 5
   その他The solvents were removed under aspirator vacuum (40-80° C.)
6. 6
   workup.DISTILLATIONThe residue was distilled under high vacuum
7. 7
   その他The 22.50 grams of the product was collected between 72-80° C. at 2 mm pressure as a clear liquid

実験手順

A mixture of 1-chloromethyl-2-methyl-2-propanol (21.80 g, 0.20 mole), sodium methacrylate (32.40 g, 0.30 mole), Adogen 464 (7.00 g, 0.015 mole) (phase transfer catalyst purchased from Aldrich Chemical Co.), and phenothiazine (60 mg) in butyronitrile (200 ml) was heated to reflux under nitrogen in a three-necked round bottomed flask equipped with a condenser and a mechanical stirrer. After cooling the contents to room temperature, the mixture was diluted with hexane (200 ml) and filtered through celite. The solvents were removed under aspirator vacuum (40-80° C.). The residue was distilled under high vacuum. The 22.50 grams of the product was collected between 72-80° C. at 2 mm pressure as a clear liquid.

出典