tert-butyl N-spiro[2.5]octan-6-ylcarbamate

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

实验步骤: Compound 7-3 (1.5 g, 6.7 mmol) was dissolved in 15 mL of DCM and TFA (2.5 mL) was added and stirred for 1 hour to give Compound 7-4 (1.6 g, 99.8% yield).

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

实验步骤: Diethyl zinc (40 mL, 1 M solution in hexane) was slowly added to 300 mL of anhydrous DCM at −78° C. under nitrogen, further dimethyl iodide (15 g, 56 mmol) was added slowly. After 30 minutes, warmed to room temperature and maintained for 30 minutes, cooled with an ice-water bath. Then a solution of Compound 7-2 (2 g, 9.5 mmol) dissolved in 10 mL of methylene chloride was added and reacted overnight. To the reaction mixture was poured 100 mL of saturated aqueous solution of ammonium chloride, and liquid separated, the organic phase was extracted with ethyl acetate (100 mL) twice, the organic phases were combined and dried over anhydrous sodium sulfate. Suction filtered to remove desiccant, and rotary evaporated to remove solvents. The residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate=10:1) to give Compound 7-3 as a white solid (0.8 g, 37.4% yield). maintained for 30 minutes cooled with an ice-water bath was added reacted overnight separated the organic phase was extracted with ethyl acetate (100 mL) twice dried over anhydrous sodium sulfate Suction filtered to remove desiccant rotary evaporated to remove solvents The residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate=10:1)