반응 #334184

반응 방정식

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

수율 22.5%

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

수율 22.5%

용매

acetonitrile

water

반응 조건

후처리

1. 1
   추출The aqueous layer was extracted with methylene chloride (3×10 mL)
2. 2
   건조The organic layer was dried (Na2SO4)
3. 3
   여과filtered
4. 4
   기타the solvent was removed with a rotary evaporator
5. 5
   기타The residue was triturated with ethyl acetate

실험 절차

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.

출처