反応 #1066146

反応方程式

2-chloro-N'-methylbenzenesulfonimidamide

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

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

HCl

→

white solid

収率 22.5%

2-Chloro-N-[(4-methoxy-6-methyl-1,3,5-triazin-2-yl)-aminocarbonyl]-N'-methylbenzenesulfonimidamide

収率 22.5%

溶媒

acetonitrile

water

反応条件

後処理

1. 1
   抽出The aqueous layer was extracted with methylene chloride (3×10 mL)
2. 2
   乾燥The organic layer was dried (Na2SO4)
3. 3
   ろ過filtered
4. 4
   その他the solvent was removed with a rotary evaporator
5. 5
   その他The residue was triturated with ethyl acetate

実験手順

To a solution of 196.8 mg (0.96 mmol) of 2-chloro-N'-methylbenzenesulfonimidamide and 250 mg (0.96 mmol) of phenyl(4-methoxy-6-methyl-1,3,5-triazin-2-yl)-carbamate in 5 mL of dry acetonitrile was added 0.15 mL (1.0 mmol) of 1,8-diazabicyclo[5.4.0]-undec-7-ene. After 45 minutes at room temperature, 5 mL of water and 2.5 mL of 5% HCl were added. The aqueous layer was extracted with methylene chloride (3×10 mL). The organic layer was dried (Na2SO4), filtered and the solvent was removed with a rotary evaporator. The residue was triturated with ethyl acetate to give 80 mg of a white solid; m.p. 154° to 160° C.

出典