tert-butyl N-(12-hydroxydodecyl)carbamate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a suspension of 0.5 g of tert-butyl N-(12-hydroxydodecyl)carbamate in 15 ml of toluene were added 0.28 g of imidazole, 1.09 g of triphenylphosphine and 0.84 g of iodine and the mixture was stirred for 0.5 hour. Then, 5 ml of tetrahydrofuran was further added and the mixture was stirred for 2 hours. To the reaction solution was added ethyl acetate and the mixture was washed successively with a 10% aqueous solution of sodium thiosulfate and water and dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The residue thus obtained was chromatographed over a silica gel column to afford 0.42 g of the title compound. the mixture was stirred for 2 hours the mixture was washed successively with a 10% aqueous solution of sodium thiosulfate and water dried over anhydrous sodium sulfate the solvent was distilled off under reduced pressure The residue thus obtained was chromatographed over a silica gel column

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a suspension of 0.5 g of tert-butyl N-(12-hydroxydodecyl)carbamate in 15 ml of toluene were added 0.28 g of imidazole, 1.09 g of triphenylphosphine and 0.84 g of iodine and the mixture was stirred for 0.5 hour. Then, 5 ml of tetrahydrofuran was further added and the mixture was stirred for 2 hours. To the reaction solution was added ethyl acetate and the mixture was washed successively with a 10% aqueous solution of sodium thiosulfate and water and dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The residue thus obtained was chromatographed over a silica gel column to afford 0.42 g of the title compound. the mixture was stirred for 2 hours the mixture was washed successively with a 10% aqueous solution of sodium thiosulfate and water dried over anhydrous sodium sulfate the solvent was distilled off under reduced pressure The residue thus obtained was chromatographed over a silica gel column

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 8.96 g of tert-butyl N-(12-hydroxydodecyl)carbamate in 60 ml of tetrahydrofuran were successively added dropwise under ice-cooling 2.1 ml of mesyl chloride and 3.8 ml of triethylamine and the mixture was stirred for one hour. To the reaction solution was added ethyl acetate and the mixture was washed successively with water, a saturated aqueous solution of sodium hydrogen carbonate, water and a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure to afford 8.06 g of the title compound. the mixture was washed successively with water a saturated aqueous solution of sodium hydrogen carbonate, water and a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate the solvent was distilled off under reduced pressure

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 8.96 g of tert-butyl N-(12-hydroxydodecyl)carbamate in 60 ml of tetrahydrofuran were successively added dropwise under ice-cooling 2.1 ml of mesyl chloride and 3.8 ml of triethylamine and the mixture was stirred for one hour. To the reaction solution was added ethyl acetate and the mixture was washed successively with water, a saturated aqueous solution of sodium hydrogen carbonate, water and a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure to afford 8.06 g of the title compound. the mixture was washed successively with water a saturated aqueous solution of sodium hydrogen carbonate, water and a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate the solvent was distilled off under reduced pressure

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a suspension of 5.0 g of tert-butyl N-(12-hydroxydodecyl)carbamate in 25 ml of methanol was added 3 ml of hydrochloric acid and the mixture was heated under reflux for one hour. The reaction solution was distilled off under reduced pressure, ethyl acetate was added to the residue, the crystal thus precipitated out was recovered by filtration and dried under reduced pressure to afford 3.23 g of the title compound. the mixture was heated under reflux for one hour The reaction solution was distilled off under reduced pressure, ethyl acetate was added to the residue the crystal thus precipitated out was recovered by filtration dried under reduced pressure

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a suspension of 0.5 g of tert-butyl N-(12-hydroxydodecyl)carbamate in 15 ml of toluene were added 0.28 g of imidazole, 1.09 g of triphenylphosphine and 0.84 g of iodine and the mixture was stirred for 0.5 hour. Then, 5 ml of tetrahydrofuran was further added and the mixture was stirred for 2 hours. To the reaction solution was added ethyl acetate and the mixture was washed successively with a 10% aqueous solution of sodium thiosulfate and water and dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The residue thus obtained was chromatographed over a silica gel column to afford 0.42 g of the title compound. the mixture was stirred for 2 hours the mixture was washed successively with a 10% aqueous solution of sodium thiosulfate and water dried over anhydrous sodium sulfate the solvent was distilled off under reduced pressure The residue thus obtained was chromatographed over a silica gel column

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 8.96 g of tert-butyl N-(12-hydroxydodecyl)carbamate in 60 ml of tetrahydrofuran were successively added dropwise under ice-cooling 2.1 ml of mesyl chloride and 3.8 ml of triethylamine and the mixture was stirred for one hour. To the reaction solution was added ethyl acetate and the mixture was washed successively with water, a saturated aqueous solution of sodium hydrogen carbonate, water and a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure to afford 8.06 g of the title compound. the mixture was washed successively with water a saturated aqueous solution of sodium hydrogen carbonate, water and a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate the solvent was distilled off under reduced pressure

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a suspension of 5.0 g of tert-butyl N-(12-hydroxydodecyl)carbamate in 25 ml of methanol was added 3 ml of hydrochloric acid and the mixture was heated under reflux for one hour. The reaction solution was distilled off under reduced pressure, ethyl acetate was added to the residue, the crystal thus precipitated out was recovered by filtration and dried under reduced pressure to afford 3.23 g of the title compound. the mixture was heated under reflux for one hour The reaction solution was distilled off under reduced pressure, ethyl acetate was added to the residue the crystal thus precipitated out was recovered by filtration dried under reduced pressure