propan-2-yl N-phenylcarbamate

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:

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

実験手順: A liquid mixture of 50 g (0.42 mol) of phenyl isocyanate and 6.43 ml (0.084 mol) of isopropanol was stirred at room temperature for 20 minutes and thereafter an unreacted raw material was distilled away under a reduced pressure to obtain 16.1% of isopropyl N-phenylcarbamate. an unreacted raw material was distilled away under a reduced pressure

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

実験手順: A liquid mixture of 50 g (0.42 mol) of phenyl isocyanate and 6.43 ml (0.084 mol) of isopropanol was stirred at room temperature for 20 minutes and thereafter an unreacted raw material was distilled away under a reduced pressure to obtain 16.1% of isopropyl N-phenylcarbamate. an unreacted raw material was distilled away under a reduced pressure

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

実験手順: Eighteen grams isopropyl phenylcarbamate (~0.1 mol) and 14.0 g thionyl chloride (0.12 mol) were dissolved in 50 ml dry tetrahydrofuran and protected from moisture by a calcium chloride tube. Eight grams pyridine (0.1 mol) were added dropwise while the mixture was stirring at a water bath temperature (15°-20° C.). After the addition of pyridine was completed, the mixture was stirred for 12 hours at room temperature. Pyridine hydrochloride was filtered and the solvent was removed under vacuum. The concentrated residue was diluted with hexane and filtered. The hexane was removed under vacuum and the residue was distilled, giving 16.0 g of product distilling at 113-115/0.08 mm. NMR spectrum of the product in chloroform-d-TMS gave the following absorptions: δ7.6-7.2 (m, 5H, phenyl protons), δ5.5-4.9 (m, 1H, CH) and δ1.4-1.3 (d, 6H, C(CH3)2). protected from moisture by a calcium chloride tube the mixture was stirred for 12 hours at room temperature Pyridine hydrochloride was filtered the solvent was removed under vacuum The concentrated residue was diluted with hexane filtered The hexane was removed under vacuum the residue was distilled

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

実験手順: Eighteen grams isopropyl phenylcarbamate (~0.1 mol) and 14.0 g thionyl chloride (0.12 mol) were dissolved in 50 ml dry tetrahydrofuran and protected from moisture by a calcium chloride tube. Eight grams pyridine (0.1 mol) were added dropwise while the mixture was stirring at a water bath temperature (15°-20° C.). After the addition of pyridine was completed, the mixture was stirred for 12 hours at room temperature. Pyridine hydrochloride was filtered and the solvent was removed under vacuum. The concentrated residue was diluted with hexane and filtered. The hexane was removed under vacuum and the residue was distilled, giving 16.0 g of product distilling at 113-115/0.08 mm. NMR spectrum of the product in chloroform-d-TMS gave the following absorptions: δ7.6-7.2 (m, 5H, phenyl protons), δ5.5-4.9 (m, 1H, CH) and δ1.4-1.3 (d, 6H, C(CH3)2). protected from moisture by a calcium chloride tube the mixture was stirred for 12 hours at room temperature Pyridine hydrochloride was filtered the solvent was removed under vacuum The concentrated residue was diluted with hexane filtered The hexane was removed under vacuum the residue was distilled

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

実験手順: A liquid mixture of 50 g (0.42 mol) of phenyl isocyanate and 6.43 ml (0.084 mol) of isopropanol was stirred at room temperature for 20 minutes and thereafter an unreacted raw material was distilled away under a reduced pressure to obtain 16.1% of isopropyl N-phenylcarbamate. an unreacted raw material was distilled away under a reduced pressure

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

実験手順: Eighteen grams isopropyl phenylcarbamate (~0.1 mol) and 14.0 g thionyl chloride (0.12 mol) were dissolved in 50 ml dry tetrahydrofuran and protected from moisture by a calcium chloride tube. Eight grams pyridine (0.1 mol) were added dropwise while the mixture was stirring at a water bath temperature (15°-20° C.). After the addition of pyridine was completed, the mixture was stirred for 12 hours at room temperature. Pyridine hydrochloride was filtered and the solvent was removed under vacuum. The concentrated residue was diluted with hexane and filtered. The hexane was removed under vacuum and the residue was distilled, giving 16.0 g of product distilling at 113-115/0.08 mm. NMR spectrum of the product in chloroform-d-TMS gave the following absorptions: δ7.6-7.2 (m, 5H, phenyl protons), δ5.5-4.9 (m, 1H, CH) and δ1.4-1.3 (d, 6H, C(CH3)2). protected from moisture by a calcium chloride tube the mixture was stirred for 12 hours at room temperature Pyridine hydrochloride was filtered the solvent was removed under vacuum The concentrated residue was diluted with hexane filtered The hexane was removed under vacuum the residue was distilled

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: