DIMETHYL(4-CHLOROPHENYLOXOMETHYL)PHOSPHONATE

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of dimethyl p-chlorobenzoylphosphonate (1 mmol) in dry dioxane (5 ml), BrMe3Si (3 mmol) was added dropwise under magnetic stirring, in nitrogen atmosphere at room temperature. After 5 hours the solvent was removed under vacuum and the brown residue was dissolved in MeOH at 0° C. The solvent was evaporated and a solution of NaOH (1 mmol) in MeOH (5 ml) was added in portions. The white solid was filtered and dried under vacuum. Yield: 76%. NMR, 1H, 7.54 (d, 2 H), 8.11 (d, 2 H); 31P, −1.48 ppm. After 5 hours the solvent was removed under vacuum the brown residue was dissolved in MeOH at 0° C The solvent was evaporated The white solid was filtered dried under vacuum

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of dimethyl p-chlorobenzoylphosphonate (1 mmol) in dry dioxane (5 ml), BrMe3Si (3 mmol) was added dropwise under magnetic stirring, in nitrogen atmosphere at room temperature. After 5 h the solvent was removed under vacuum and the brown residue was dissolved in MeOH at 0° C. The solvent was evaporated and a solution of NaOH (1 mmol) in MeOH (5 ml) was added in portions. The white solid was filtered and dried under vacuum. Yield: 76%. NMR, 1H: 7.54 (d, 2H), 8.11 (d, 2H); 31P, −1.48 ppm. After 5 h the solvent was removed under vacuum the brown residue was dissolved in MeOH at 0° C The solvent was evaporated The white solid was filtered dried under vacuum

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of dimethyl p-chlorobenzoylphosphonate (1 mmol) in dry dioxane (5 ml), BrMe3Si (3 mmol) was added dropwise under magnetic stirring, in nitrogen atmosphere at room temperature. After 5 h the solvent was removed under vacuum and the brown residue was dissolved in MeOH at 0° C. The solvent was evaporated and a solution of NaOH (1 mmol) in MeOH (5 ml) was added in portions. The white solid was filtered and dried under vacuum. Yield: 76%. NMR, 1H: 7.54 (d, 2H), 8.11 (d, 2H); 31P, −1.48 ppm. After 5 h the solvent was removed under vacuum the brown residue was dissolved in MeOH at 0° C The solvent was evaporated The white solid was filtered dried under vacuum

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of dimethyl p-chlorobenzoylphosphonate (1 mmol) in dry dioxane (5 ml), BrMe3Si (3 mmol) was added dropwise under magnetic stirring, in nitrogen atmosphere at room temperature. After 5 h the solvent was removed under vacuum and the brown residue was dissolved in MeOH at 0° C. The solvent was evaporated and a solution of NaOH (1 mmol) in MeOH (5 ml) was added in portions. The white solid was filtered and dried under vacuum. Yield: 76%. NMR, 1H: 7.54 (d, 2H), 8.11 (d, 2H); 31P, −1.48 ppm. After 5 h the solvent was removed under vacuum the brown residue was dissolved in MeOH at 0° C The solvent was evaporated The white solid was filtered dried under vacuum