反应详情

Route with additives: In a test tube the mixture of 1 ml (2.95 mmol) of methyl oleate, the corresponding amount of 2-butene-1,4-diol (0.24 ml or 0.73 ml) and 0.1 ml of tetradecane (internal standard) is prepared and mixed. If the reaction is being carried out without solvent, a blank sample is taken for GC measurement. In the case of the procedure with solvent, a blank sample for GC measurement is taken only after the addition of 1 ml of the corresponding solvent. After sampling has taken place, the test tube is placed in the thermally conditioned oil bath. The mixture is stirred for about 2 minutes using a magnetic stirrer. When the desired temperature of the mixture has been reached, the catalyst (2 mol %) is added. The reaction mixture is heated and stirred for 4 hours more. After 4 hours of reaction the next GC sample is taken. After sampling has taken place, the corresponding additive is added. The additives used were sodium hydride and tributylamine (respectively 1 and 10 mol %, based on the catalyst). After 24 hours the final GC sample is taken and the reaction is halted by addition of 1 ml of ethyl vinyl ether.

1. additionmixed
2. aliquotAfter sampling
3. additionthe catalyst (2 mol %) is added
4. temperatureThe reaction mixture is heated
5. stirringstirred for 4 hours more
6. customAfter 4 hours of reaction the next GC sample
7. aliquotAfter sampling
8. additionthe corresponding additive is added
9. waitAfter 24 hours the final GC sample is taken