morpholine-4-sulfonamide

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:

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: Morpholine (5 ml) and sulfamide (11 g) in 1,4-dioxane (100 ml) were heated at reflux for 48 h. The solvent was evaporated under reduced pressure and the resulting solid partitioned between EtOAc and water. The organic phase was collected and the aqueous phase was further extracted with EtOAc (×4). The combined organic extracts were dried (MgSO4) and the solvent removed in vacuo. The solid residue was triturated with Et2O and filtered to give the subtitle compound as a white crystallin solid. Yield: 2.1 g. at reflux for 48 h The solvent was evaporated under reduced pressure the resulting solid partitioned between EtOAc and water The organic phase was collected the aqueous phase was further extracted with EtOAc (×4) The combined organic extracts were dried (MgSO4) the solvent removed in vacuo The solid residue was triturated with Et2O filtered

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: When a mixture of equimolar quantities of phenyl diphenylphosphinite, acetaldehyde, and morpholinosulfonylamine in chlorobenzene is treated by the procedure used in the preceding experiment, the product is a white solid, mp 215°-217° C., 31P nmr (DMSO-d6) -30.9 ppm. is treated by the procedure

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

実験手順: When a mixture of equimolar quantities of phenyl diphenylphosphinite, acetaldehyde, and morpholinosulfonylamine in chlorobenzene is treated by the procedure used in the preceding experiment, the product is a white solid, mp 215°-217° C., 31P nmr (DMSO-d6) -30.9 ppm. is treated by the procedure

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

実験手順: When a mixture of equimolar quantities of phenyl diphenylphosphinite, acetaldehyde, and morpholinosulfonylamine in chlorobenzene is treated by the procedure used in the preceding experiment, the product is a white solid, mp 215°-217°C., 31P nmr (DMSO-d6) -30.9 ppm. is treated by the procedure

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 0.15 mole each of triphenyl phosphite, acetaldehyde, and morpholinosulfonylamine in 100g of chlorobenzene is warmed at 100°C. for 1.25 hrs, and the reaction mixture is stripped to 110°/0.15mm. The cooled residue is diluted with 100ml of ether, causing separation of 34.5g of crude solid product. Recrystallization of a portion from isopropyl alcohol gives a white solid, mp 104.5°-108°, 31 p nmr(DMSO-d6) -18.1 ppm. is stripped to 110° separation of 34.5g of crude solid product Recrystallization of a portion from isopropyl alcohol gives a white solid, mp 104.5°-108°, 31 p nmr(DMSO-d6) -18.1 ppm

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 0.15 mole each of triphenyl phosphite, acetaldehyde, and morpholinosulfonylamine in 100g of chlorobenzene is warmed at 100°C. for 1.25 hrs, and the reaction mixture is stripped to 110°/0.15mm. The cooled residue is diluted with 100ml of ether, causing separation of 34.5g of crude solid product. Recrystallization of a portion from isopropyl alcohol gives a white solid, mp 104.5°-108°, 31 p nmr(DMSO-d6) -18.1 ppm. is stripped to 110° separation of 34.5g of crude solid product Recrystallization of a portion from isopropyl alcohol gives a white solid, mp 104.5°-108°, 31 p nmr(DMSO-d6) -18.1 ppm