반응 #833531

반응 방정식

1-chloromethyl-2-methyl-2-propanol

sodium methacrylate

phenothiazine

→

2-hydroxy-2,2-dimethylethyl methacrylate

용매

hexane

butyronitrile

반응 조건

후처리

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

실험 절차

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.

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