反応 #1752685

反応方程式

1-(4-aminophenyl)ethanol

triphosgene

Et3N

4-(4,6-dimorpholin-4-yl-1,3,5-triazin-2-yl)aniline

→

[4-(4,6-dimorpholin-4-yl-1,3,5-triazin-2-yl)phenyl]-3-[4-(1-hydroxyethyl)phenyl]urea

収率 24.0%

溶媒

methylene chloride

反応条件

後処理

1. 1
   workup.STIRRINGThe reaction mixture was stirred for about 16 hours at room temperature
2. 2
   その他The solvent was removed
3. 3
   workup.DISSOLUTIONThe residue was dissolved in DMSO

実験手順

To a stirred mixture of 4-(4,6-dimorpholin-4-yl-1,3,5-triazin-2-yl)aniline (0.140, 0.40 mmoles) in methylene chloride at 0° C. was added triphosgene (0.25, 0.84 mmoles) and Et3N (3 mL). The reaction mixture was stirred for 20 minutes at 0° C. Then 1-(4-aminophenyl)ethanol (0.10 g, 0.73 mmoles) was added to the mixture. The reaction mixture was stirred for about 16 hours at room temperature. The solvent was removed. The residue was dissolved in DMSO and place at HPLC using acetonitrile buffer TFA to give 48 mg (24%) of [4-(4,6-dimorpholin-4-yl-1,3,5-triazin-2-yl)phenyl]-3-[4-(1-hydroxyethyl)phenyl]urea. M+H 506.4.

出典