反応 #2346374

反応方程式

HCl

Methyl 2-(aminosulfonyl)-1-methyl-1H-pyrrole-3-carboxylate

phenyl (4-methoxy-6-methyl-1,3,5-triazin-2-yl)carbamate

DBU

→

title compound

収率 73.5%

Methyl 2-[[[[(4-Methoxy-6-methyl-1,3,5-triazin-2-yl)amino]carbonyl]amino]sulfonyl]-1-methyl-1H-pyrrole-3-carboxylate

収率 73.5%

溶媒

water

acetonitrile

反応条件

後処理

1. 1
   ろ過the resulting precipitate was collected by filtration
2. 2
   洗浄rinsed successively with water and ether
3. 3
   その他dried

実験手順

Methyl 2-(aminosulfonyl)-1-methyl-1H-pyrrole-3-carboxylate (0.10 g, 0.46 mmol) and 0.13 g (0.50 mmol) of phenyl (4-methoxy-6-methyl-1,3,5-triazin-2-yl)carbamate were combined in 2 mL of acetonitrile and 0.075 mL of DBU was added and the resulting amber solution was stirred at ambient temperature for 30 min. The reaction mixture was diluted with 15 mL of water and acidified with 0.5 mL 1N HCl and the resulting precipitate was collected by filtration and rinsed successively with water and ether, then dried to afford 0.13 g of the title compound as a white solid, m.p. 189°-190° C. (dec). 1H NMR (Me2SO-d6, 200 MHz.) δ: 12.5 (NH), 11.1 (NH), 7.22 (d,1H), 6.60 (d,1H), 4.01 (s,3H), 3.98 (s,3H), 3.71 (s,3H), 2.49 (s,3H).

出典