反応 #1795112

反応方程式

HCl

3,4-dihydro-1-oxo-1H-pyrrolo[2,1-c][1,4]oxazine-8-sulfonamide

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

1,8-diazabicyclo[5.4.0]undec-7-ene

→

title compound

収率 56.5%

3,4-Dihydro-N-[[(4-methoxy-6-methyl-1,3,5-triazin-2-yl)amino]carbonyl]-1-oxo-1H-pyrrolo[2,1-c][1,4]-oxazine-8-sulfonamide

収率 56.5%

溶媒

Water

acetonitrile

ethyl ether

反応条件

後処理

1. 1
   workup.STIRRINGwith stirring
2. 2
   その他The product crystallized from the two phase mixture
3. 3
   ろ過was collected by filtration

実験手順

A solution of 40 mg (0.185 mmol) of 3,4-dihydro-1-oxo-1H-pyrrolo[2,1-c][1,4]oxazine-8-sulfonamide and 53 mg (0.204 mmol) of phenyl (4-methoxy-6-methyl-1,3,5-triazin-2-yl)carbamate in 0.8 mL acetonitrile was treated with 0.03 mL 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) and then stirred 40 minutes at ambient temperature. Water (5 mL) plus 0.5 mL 1N HCl was added with stirring followed by ca. 1 mL of ethyl ether. The product crystallized from the two phase mixture and was collected by filtration to afford 40 mg of the title compound, m.p. 204°-207° C. dec.

出典