异丁酸异丁酯

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Step 1 To a solution of diisopropylamine (2.94 mL, 20.8 mmol) in THF (20 mL) under nitrogen at 0° C. was added nBuLi (2.5M in hexanes, 8.32 mL, 20.8 mmol, 1 eq.) and the solution stirred at 0° C. for 30 min. The solution was cooled to −78° C. and then a solution of isobutylisobutyrate (3.49 mL, 20.8 mmol) in THF (6 mL) was added dropwise and then the reaction stirred at −78° C. for 1 h. TMS-Cl (3.19 mL, 25 mmol) was then added dropwise and the reaction allowed to warm to room temperature over 3 h. The reaction was quenched with ice-water (20 mL) and EtOAc (20 mL) was added. The organic phase was washed with water (10 mL) and then brine (10 mL) before it was dried (MgSO4), filtered and concentrated to give (1-isobutoxy-2-methyl-propenyloxy)-trimethyl-silane (3.5 g) used crude in the next reaction. The solution was cooled to −78° C. the reaction stirred at −78° C. for 1 h to warm to room temperature over 3 h The reaction was quenched with ice-water (20 mL) and EtOAc (20 mL) was added The organic phase was washed with water (10 mL) brine (10 mL) before it was dried (MgSO4) filtered concentrated

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Step 1 To a solution of diisopropylamine (2.94 mL, 20.8 mmol) in THF (20 mL) under nitrogen at 0° C. was added nBuLi (2.5M in hexanes, 8.32 mL, 20.8 mmol, 1 eq.) and the solution stirred at 0° C. for 30 min. The solution was cooled to −78° C. and then a solution of isobutylisobutyrate (3.49 mL, 20.8 mmol) in THF (6 mL) was added dropwise and then the reaction stirred at −78° C. for 1 h. TMS-Cl (3.19 mL, 25 mmol) was then added dropwise and the reaction allowed to warm to room temperature over 3 h. The reaction was quenched with ice-water (20 mL) and EtOAc (20 mL) was added. The organic phase was washed with water (10 mL) and then brine (10 mL) before it was dried (MgSO4), filtered and concentrated to give (1-isobutoxy-2-methyl-propenyloxy)-trimethyl-silane (3.5 g) used crude in the next reaction. The solution was cooled to −78° C. the reaction stirred at −78° C. for 1 h to warm to room temperature over 3 h The reaction was quenched with ice-water (20 mL) and EtOAc (20 mL) was added The organic phase was washed with water (10 mL) brine (10 mL) before it was dried (MgSO4) filtered concentrated