2-碘甲基苯甲酸甲酯

反应条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of the ketone (10.0 g, 32.6 mmol) of Step 1 and the iodide (2.7 g, 47.7 mmol) of Step 2 in THF was added 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (4 mL). The ketone was dissolved by heating and the resulting solution was cooled to -60° C. A solution of 0.35M lithium diisopropylamide (89.7 mL, 30.9 mmol) was then added dropwise. After the addition was completed, the dry ice bath was removed and the reaction was allowed to warm to +10° C. The reaction was quenched by the addition of 25% aq. NH4OAc and the desired product was extracted with EtOAc, dried over Na2SO4 and evaporated under reduced pressure. The resulting mixture was purified by flash chromatography (toluene to 5% EtOAc in toluene) to yield 8 g (55%) of the title product. by heating After the addition the dry ice bath was removed to warm to +10° C The reaction was quenched by the addition of 25% aq. NH4OAc the desired product was extracted with EtOAc dried over Na2SO4 evaporated under reduced pressure The resulting mixture was purified by flash chromatography (toluene to 5% EtOAc in toluene)

反应条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of the ketone (10.0 g, 32.6 mmol) of Step 1 and the iodide (2.7 g, 47.7 mmol) of Step 2 in THF was added 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (4 mL). The ketone was dissolved by heating and the resulting solution was cooled to -60° C. A solution of 0.35M lithium diisopropylamide (89.7 mL, 30.9 mmol) was then added dropwise. After the addition was completed, the dry ice bath was removed and the reaction was allowed to warm to +10° C. The reaction was quenched by the addition of 25% aq. NH4OAc and the desired product was extracted with EtOAc, dried over Na2SO4 and evaporated under reduced pressure. The resulting mixture was purified by flash chromatography (toluene to 5% EtOAc in toluene) to yield 8 g (55%) of the title product. by heating After the addition the dry ice bath was removed to warm to +10° C The reaction was quenched by the addition of 25% aq. NH4OAc the desired product was extracted with EtOAc dried over Na2SO4 evaporated under reduced pressure The resulting mixture was purified by flash chromatography (toluene to 5% EtOAc in toluene)

反应条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of the ketone (10.0 g, 32.6 mmol) of Step 1 and the iodide (2.7 g, 47.7 mmol) of Step 2 in THF was added 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (4 mL). The ketone was dissolved by heating and the resulting solution was cooled to -60° C. A solution of 0.35M lithium diisopropylamide (89.7 mL, 30.9 mmol) was then added dropwise. After the addition was completed, the dry ice bath was removed and the reaction was allowed to warm to +10° C. The reaction was quenched by the addition of 25% aq. NH4OAc and the desired product was extracted with EtOAc, dried over Na2SO4 and evaporated under reduced pressure. The resulting mixture was purified by flash chromatography (toluene to 5% EtOAc in toluene) to yield 8 g (55%) of the title product. by heating After the addition the dry ice bath was removed to warm to +10° C The reaction was quenched by the addition of 25% aq. NH4OAc the desired product was extracted with EtOAc dried over Na2SO4 evaporated under reduced pressure The resulting mixture was purified by flash chromatography (toluene to 5% EtOAc in toluene)

反应条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of the ketone (10.0 g, 32.6 mmol) of Step 1 and the iodide (2.7 g, 47.7 mmol) of Step 2 in THF was added 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (4 mL). The ketone was dissolved by heating and the resulting solution was cooled to -60° C. A solution of 0.35M lithium diisopropylamide (89.7 mL, 30.9 mmol) was then added dropwise. After the addition was completed, the dry ice bath was removed and the reaction was allowed to warm to +10° C. The reaction was quenched by the addition of 25% aq. NH4OAc and the desired product was extracted with EtOAc, dried over Na2SO4 and evaporated under reduced pressure. The resulting mixture was purified by flash chromatography (toluene to 5% EtOAc in toluene) to yield 8 g (55%) of the title product. by heating After the addition the dry ice bath was removed to warm to +10° C The reaction was quenched by the addition of 25% aq. NH4OAc the desired product was extracted with EtOAc dried over Na2SO4 evaporated under reduced pressure The resulting mixture was purified by flash chromatography (toluene to 5% EtOAc in toluene)

反应条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of the ketone (10.0 g, 32.6 mmol) of Step 1 and the iodide (2.7 g, 47.7 mmol) of Step 2 in THF was added 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (4 mL). The ketone was dissolved by heating and the resulting solution was cooled to -60° C. A solution of 0.35M lithium diisopropylamide (89.7 mL, 30.9 mmol) was then added dropwise. After the addition was completed, the dry ice bath was removed and the reaction was allowed to warm to +10° C. The reaction was quenched by the addition of 25% aq. NH4OAc and the desired product was extracted with EtOAc, dried over Na2SO4 and evaporated under reduced pressure. The resulting mixture was purified by flash chromatography (toluene to 5% EtOAc in toluene) to yield 8 g (55%) of the title product. by heating After the addition the dry ice bath was removed to warm to +10° C The reaction was quenched by the addition of 25% aq. NH4OAc the desired product was extracted with EtOAc dried over Na2SO4 evaporated under reduced pressure The resulting mixture was purified by flash chromatography (toluene to 5% EtOAc in toluene)

反应条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of the ketone (10.0 g, 32.6 mmol) of Step 1 and the iodide (2.7 g, 47.7 mmol) of Step 2 in THF was added 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (4 mL). The ketone was dissolved by heating and the resulting solution was cooled to -60° C. A solution of 0.35M lithium diisopropylamide (89.7 mL, 30.9 mmol) was then added dropwise. After the addition was completed, the dry ice bath was removed and the reaction was allowed to warm to +10° C. The reaction was quenched by the addition of 25% aq. NH4OAc and the desired product was extracted with EtOAc, dried over Na2SO4 and evaporated under reduced pressure. The resulting mixture was purified by flash chromatography (toluene to 5% EtOAc in toluene) to yield 8 g (55%) of the title product. by heating After the addition the dry ice bath was removed to warm to +10° C The reaction was quenched by the addition of 25% aq. NH4OAc the desired product was extracted with EtOAc dried over Na2SO4 evaporated under reduced pressure The resulting mixture was purified by flash chromatography (toluene to 5% EtOAc in toluene)

反应条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of the ketone (10.0 g, 32.6 mmol) of Step 1 and the iodide (2.7 g, 47.7 mmol) of Step 2 in THF was added 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (4 mL). The ketone was dissolved by heating and the resulting solution was cooled to -60° C. A solution of 0.35M lithium diisopropylamide (89.7 mL, 30.9 mmol) was then added dropwise. After the addition was completed, the dry ice bath was removed and the reaction was allowed to warm to +10° C. The reaction was quenched by the addition of 25% aq. NH4OAc and the desired product was extracted with EtOAc, dried over Na2SO4 and evaporated under reduced pressure. The resulting mixture was purified by flash chromatography (toluene to 5% EtOAc in toluene) to yield 8 g (55%) of the title product. by heating After the addition the dry ice bath was removed to warm to +10° C The reaction was quenched by the addition of 25% aq. NH4OAc the desired product was extracted with EtOAc dried over Na2SO4 evaporated under reduced pressure The resulting mixture was purified by flash chromatography (toluene to 5% EtOAc in toluene)