N-(2-hydroxyethyl)-2-[[1-(2-hydroxyethylamino)-2-methyl-1-oxopropan-2-yl]diazenyl]-2-methylpropanamide

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

実験手順: Thionyl chloride (50 ml) was added at 0° C. under an atmosphere of inert gas (argon) to a suspension of 2,2′-azobis[2-methyl-N-(2-hydroxyethyl)propionamide] (38.3 g) in dichloromethane (180 ml) over a period of 30 minutes. The mixture was stirred at room temperature for 18 h, and the precipitate which formed was filtered off, suspended in 100 ml of water and stirred for 5 min. The solid was separated off and dried under reduced pressure at room temperature for 24 h (8.9 g). Further product was isolated from the organic phase of the reaction mixture by adding cyclohexane (250 ml) and cooling to 0° C. The precipitate which formed was filtered off, and worked up and isolated as described above (10.8 g). Finally, the remaining organic filtrate was concentrated to low volume. The precipitate which formed was subjected to the procedure described above (7.6 g). the precipitate which formed was filtered off stirred for 5 min The solid was separated off dried under reduced pressure at room temperature for 24 h (8.9 g) Further product was isolated from the organic phase of the reaction mixture cooling to 0° C The precipitate which formed was filtered off isolated Finally, the remaining organic filtrate was concentrated to low volume The precipitate which formed

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

実験手順: Thionyl chloride (50 ml) was added at 0° C. under an atmosphere of inert gas (argon) to a suspension of 2,2′-azobis[2-methyl-N-(2-hydroxyethyl)propionamide] (38.3 g) in dichloromethane (180 ml) over a period of 30 minutes. The mixture was stirred at room temperature for 18 h, and the precipitate which formed was filtered off, suspended in 100 ml of water and stirred for 5 min. The solid was separated off and dried under reduced pressure at room temperature for 24 h (8.9 g). Further product was isolated from the organic phase of the reaction mixture by adding cyclohexane (250 ml) and cooling to 0° C. The precipitate which formed was filtered off, and worked up and isolated as described above (10.8 g). Finally, the remaining organic filtrate was concentrated to low volume. The precipitate which formed was subjected to the procedure described above (7.6 g). the precipitate which formed was filtered off stirred for 5 min The solid was separated off dried under reduced pressure at room temperature for 24 h (8.9 g) Further product was isolated from the organic phase of the reaction mixture cooling to 0° C The precipitate which formed was filtered off isolated Finally, the remaining organic filtrate was concentrated to low volume The precipitate which formed

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

実験手順: Thionyl chloride (50 ml) was added at 0° C. under an atmosphere of inert gas (argon) to a suspension of 2,2′-azobis[2-methyl-N-(2-hydroxyethyl)propionamide] (38.3 g) in dichloromethane (180 ml) over a period of 30 minutes. The mixture was stirred at room temperature for 18 h, and the precipitate which formed was filtered off, suspended in 100 ml of water and stirred for 5 min. The solid was separated off and dried under reduced pressure at room temperature for 24 h (8.9 g). Further product was isolated from the organic phase of the reaction mixture by adding cyclohexane (250 ml) and cooling to 0° C. The precipitate which formed was filtered off, and worked up and isolated as described above (10.8 g). Finally, the remaining organic filtrate was concentrated to low volume. The precipitate which formed was subjected to the procedure described above (7.6 g). the precipitate which formed was filtered off stirred for 5 min The solid was separated off dried under reduced pressure at room temperature for 24 h (8.9 g) Further product was isolated from the organic phase of the reaction mixture cooling to 0° C The precipitate which formed was filtered off isolated Finally, the remaining organic filtrate was concentrated to low volume The precipitate which formed