放线醇

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

实验步骤: 300 g of (4R, 6R)-4-hydroxy-2,2,6-trimethylcyclohexanone were dissolved in 154.7 ml of pyridine. The solution was treated dropwise at -3° C. to 0° C. within 10 minutes with 1.2 l of acetic anhydride and then stirred at room temperature for a further 4.25 hours. The reaction mixture was subsequently concentrated on a rotary evaporator at 60° C./16 mbar, whereby there were obtained 394.7 g of crude product as a yellow oil. Distillation of the crude product gave at about 95° C./0.07 mbar 378.4 g (99.4%) of (4R, 6R)-4-acetoxy-2,2,6-trimethylcyclohexanone as a colourless oil. The reaction mixture was subsequently concentrated on a rotary evaporator at 60° C./16 mbar whereby there were obtained 394.7 g of crude product as a yellow oil Distillation of the crude product

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

实验步骤: 0.79 g (6.86 mmol) of potassium tert-butoxide (KOtBu) was added to a solution of 2.5 g (6.86 mmol) of methyltriphenylphosphonium bromide in 10 ml of dimethyl sulfoxide (DMSO) under N2, and the mixture was then stirred at RT for 30 min. 0.36 g (2.29 mmol) of (4R,6R)-4-hydroxy-2,2,6-trimethyl-1-cyclohexanone was added to this mixture, which was then stirred at RT for 5 min. during which a white precipitate appeared. The mixture was then stirred at 60° C. for 15 min, cooled to RT, poured into 150 ml of ice-water and extracted twice with 50 ml of methylene chloride. The organic phase was separated off, washed with 50 ml of a 5% strength aqueous Na2CO3 solution and 50 ml of water and dried over MgSO4, and the solvent was removed under reduced pressure. was then stirred at RT for 5 min. during which a white precipitate The mixture was then stirred at 60° C. for 15 min cooled to RT extracted twice with 50 ml of methylene chloride The organic phase was separated off washed with 50 ml of a 5% strength aqueous Na2CO3 solution and 50 ml of water dried over MgSO4 the solvent was removed under reduced pressure

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

实验步骤: 300 g of (4R,6R)-4-hydroxy-2,2,6-trimethylcyclohexanone were dissolved in 154.7 ml of pyridine. The solution was treated dropwise at -3° C. to 0° C. within 10 minutes with 1.2 l of acetic anhydride and then stirred at room temperature for a further 4.25 hours. The reaction mixture was subsequently concentrated on a rotary evaporator at 60° C./16 mbar, whereby there were obtained 394.7 g of crude product as a yellow oil. Distillation of the crude product gave at about 95° C./0.07 mbar 378.4 g (99.4%) of (4R,6R)-4-acetoxy-2,2,6-trimethylcyclohexanone as a colourless oil. The reaction mixture was subsequently concentrated on a rotary evaporator at 60° C./16 mbar whereby there were obtained 394.7 g of crude product as a yellow oil Distillation of the crude product

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

实验步骤: 300 g of (4R, 6R)-4-hydroxy-2,2,6-trimethylcyclohexanone were dissolved in 154.7 ml of pyridine. The solution was treated dropwise at -3° C. to 0° C. within 10 minutes with 1.2 l of acetic anhydride and then stirred at room temperature for a further 4.25 hours. The reaction mixture was subsequently concentrated on a rotary evaporator at 60° C./16 mbar, whereby there were obtained 394.7 g of crude product as a yellow oil. Distillation of the crude product gave at about 95° C./0.07 mbar 378.4 g (99.4%) of (4R, 6R)-4-acetoxy-2,2,6-trimethylcyclohexanone as a colourless oil. The reaction mixture was subsequently concentrated on a rotary evaporator at 60° C./16 mbar whereby there were obtained 394.7 g of crude product as a yellow oil Distillation of the crude product