反応 #2490105

反応方程式

CDI

Z-Glu-OBn

2-amino-4-chlorophenol-6-sulfonic acid

THF

→

title compound

収率 40.0%

N5-(2-hydroxy-3-sulfophenyl)-L-glutamine

収率 40.0%

溶媒

methylene chloride

反応条件

後処理

1. 1
   workup.STIRRINGstirred overnight at room temperature
2. 2
   その他After removing
3. 3
   その他a solvent, purification
4. 4
   workup.DISSOLUTIONThe obtained intermediate was dissolved in a mixed solvent of methanol and water
5. 5
   workup.ADDITIONPd/C in catalyst quantity was added
6. 6
   workup.STIRRINGstirred under hydrogen atmosphere overnight at room temperature
7. 7
   ろ過After filtering out the catalyst
8. 8
   その他removing
9. 9
   その他a solvent, purification

実験手順

Z-Glu-OBn (371 mg, 1 mmol) was dissolved in methylene chloride (1 mL), and CDI (180 mg, 1.1 mmol) was added thereto and stirred at room temperature for 30 minutes. Then, 2-amino-4-chlorophenol-6-sulfonic acid (223 mg, 1 mmol) and THF (1 mL) were added thereto and stirred overnight at room temperature. After removing a solvent, purification was conducted in accordance with the purification process A. The obtained intermediate was dissolved in a mixed solvent of methanol and water. Pd/C in catalyst quantity was added thereto and stirred under hydrogen atmosphere overnight at room temperature. After filtering out the catalyst and removing a solvent, purification was conducted in accordance with the purification process A to obtain a title compound.

出典