反应详情

In a flask, Mg (5.7 g) was placed in THF (50 mL) with an iodine chip. The reaction mixture was vigorously stirred and heated slightly, as 4-bromobutene (25 mL) was added. After consumption of Mg metal, the resulting solution was cannulated into a flask containing a mixture of [1-cyano-2-(tetrahydro-pyran-4-yl)-vinyl]-phosphonic acid diethyl ester (21.78 g, 79.7 mmol), prepared as described in Example 1 Step D above, and CuI (0.3 g) with THF (30 mL). The resulting mixture was stirred for three hours. Saturated aqueous NH4Cl solution and ethyl acetate were then added. The organic layer was separated and dried with MgSO4, filtered, and evaporated in vacuo to yield an oil.

1. additionwas added
2. customAfter consumption of Mg metal
3. customthe resulting solution was cannulated into a flask
4. additioncontaining
5. customprepared
6. stirringThe resulting mixture was stirred for three hours
7. customThe organic layer was separated
8. dry with materialdried with MgSO4
9. filtrationfiltered
10. customevaporated in vacuo
11. customto yield an oil