反応 #88021

反応方程式

methyl 3-(N-methylsulfamoyl)thiophene-2-carboxylate

K2CO3

4-(2-chloroethyl)morpholine hydrochloride

→

methyl 3-(N-methyl-N-(2-morpholinoethyl)sulfamoyl)thiophene-2-carboxylate

溶媒

DMF

反応条件

後処理

1. 1
   その他the mixture was reacted at 60° C. overnight
2. 2
   ろ過The insoluble inorganic salts were filtered off
3. 3
   その他the filtrate was evaporated
4. 4
   その他the residue was purified by flash chromatography on silica gel (DCM/MeOH=9/1)

実験手順

To a solution of methyl 3-(N-methylsulfamoyl)thiophene-2-carboxylate (prepared in an analogous manner as described in Example 10, Scheme 10, Step 1, 530 mg, 2.253 mmol) in dry DMF (20 ml) under nitrogen atmosphere, K2CO3 (623 mg, 4.51 mmol) and 4-(2-chloroethyl)morpholine hydrochloride (838 mg, 4.51 mmol) were added, and the mixture was reacted at 60° C. overnight and then at 80° C. for 5 hours. The insoluble inorganic salts were filtered off, the filtrate was evaporated and the residue was purified by flash chromatography on silica gel (DCM/MeOH=9/1) to afford methyl 3-(N-methyl-N-(2-morpholinoethyl)sulfamoyl)thiophene-2-carboxylate (Int. 47) (510 mg, 1.464 mmol, MS/ESI+348.8 [MH]+).

出典