1-(4-氟苯基)-2-甲氧基乙烷-1-胺

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a microwave vial equipped with a stir bar was added 1-(4-fluorophenyl)-2-methoxyethanamine (1.2 g, 7.09 mmol) and water (10 mL). To this mixture was added HCl (1N, 7.23 mL, 7.23 mmol) and potassium cyanate (2.88 g, 35.5 mmol). The mixture was heated in a microwave reactor to 80° C. for 1 h. Saturated sodium bicarbonate was added and the products extracted into EtOAc (×4). The organic layers were combined, washed with brine (×2), and dried over MgSO4. The material was concentrated in vacuo while loading onto silica gel. Purification by flash chromatography (0-10% EtOAc-Hexanes) gave 1-(1-(4-fluorophenyl)-2-methoxyethyl)urea. MS ESI calc'd. for C10H13FN2O2 [M+1]+ 213. found 213. To a microwave vial equipped with a stir bar the products extracted into EtOAc (×4) washed with brine (×2) dried over MgSO4 The material was concentrated in vacuo Purification by flash chromatography (0-10% EtOAc-Hexanes)

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a microwave vial equipped with a stir bar was added 1-(4-fluorophenyl)-2-methoxyethanamine (1.2 g, 7.09 mmol) and water (10 mL). To this mixture was added HCl (1N, 7.23 mL, 7.23 mmol) and potassium cyanate (2.88 g, 35.5 mmol). The mixture was heated in a microwave reactor to 80° C. for 1 h. Saturated sodium bicarbonate was added and the products extracted into EtOAc (×4). The organic layers were combined, washed with brine (×2), and dried over MgSO4. The material was concentrated in vacuo while loading onto silica gel. Purification by flash chromatography (0-10% EtOAc-Hexanes) gave 1-(1-(4-fluorophenyl)-2-methoxyethyl)urea. MS ESI calc'd. for C10H13FN2O2 [M+1]+ 213. found 213. To a microwave vial equipped with a stir bar the products extracted into EtOAc (×4) washed with brine (×2) dried over MgSO4 The material was concentrated in vacuo Purification by flash chromatography (0-10% EtOAc-Hexanes)

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a microwave vial equipped with a stir bar was added 1-(4-fluorophenyl)-2-methoxyethanamine (1.2 g, 7.09 mmol) and water (10 mL). To this mixture was added HCl (1N, 7.23 mL, 7.23 mmol) and potassium cyanate (2.88 g, 35.5 mmol). The mixture was heated in a microwave reactor to 80° C. for 1 h. Saturated sodium bicarbonate was added and the products extracted into EtOAc (×4). The organic layers were combined, washed with brine (×2), and dried over MgSO4. The material was concentrated in vacuo while loading onto silica gel. Purification by flash chromatography (0-10% EtOAc-Hexanes) gave 1-(1-(4-fluorophenyl)-2-methoxyethyl)urea. MS ESI calc'd. for C10H13FN2O2 [M+1]+ 213. found 213. To a microwave vial equipped with a stir bar the products extracted into EtOAc (×4) washed with brine (×2) dried over MgSO4 The material was concentrated in vacuo Purification by flash chromatography (0-10% EtOAc-Hexanes)