반응 #88021

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

K2CO3

4-(2-chloroethyl)morpholine hydrochloride

→

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

용매

DMF

반응 조건

후처리

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

실험 절차

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]+).

출처