Reaktion #1076756

Reaktionsgleichung

( 1 )

Phe-Gly-OBn

N-methylmorpholine

Trt-Gly-Gly

N-hydroxysuccinimide

DCC

→

Trt-Gly-Gly-Phe-Gly-OBz

Lösungsmittel

DMF

DMF

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigea reaction at 4° C. for 3 hours
2. 2
   Sonstigeto thereby obtain a reaction mixture
3. 3
   SonstigeTo the obtained reaction mixture
4. 4
   Sonstigea reaction at 4° C. for 15 hours
5. 5
   Sonstigeto thereby obtain a reaction mixture
6. 6
   SonstigeA precipitate contained in the obtained reaction mixture
7. 7
   Sonstigewas removed
8. 8
   Sonstigethe resultant solution was evaporated to dryness
9. 9
   Sonstigeto thereby obtain a residue
10. 10
    SonstigeThe obtained residue was purified by silica gel column chromatography (silica gel: Art No. 9365, Silica gel 60, 200-400 mesh, manufactured and sold by E. Merck, Darmstadt, Germany, eluent: chloroform/methanol=20/1)

Vorschrift

To 10 ml of dry DMF were added 1.54 g of Trt-Gly-Gly, 0.52 g of N-hydroxysuccinimide and 0.93 g of DCC, followed by effecting a reaction at 4° C. for 3 hours, to thereby obtain a reaction mixture. To the obtained reaction mixture was added a DMF solution containing 2.0 g of Phe-Gly-OBn para-toluenesulfonate synthesized in item (1) and 0.41 g of N-methylmorpholine, which are dissolved in 10 ml of DMF, followed by effecting a reaction at 4° C. for 15 hours, to thereby obtain a reaction mixture. A precipitate contained in the obtained reaction mixture was removed and the resultant solution was evaporated to dryness, to thereby obtain a residue. The obtained residue was purified by silica gel column chromatography (silica gel: Art No. 9365, Silica gel 60, 200-400 mesh, manufactured and sold by E. Merck, Darmstadt, Germany, eluent: chloroform/methanol=20/1), to thereby obtain 1.5 g of Trt-Gly-Gly-Phe-Gly-OBz.

Quelle