Reaktion #500400

Reaktionsgleichung

product

(2S)-2-(1-Adamantylmethoxycarbonylamino)-3-((5-(2-(1,4,5,6-tetrahydropyrimidin-2-ylcarbamoyl)-cyclopropyl)-thiophene-2-carbonyl)-amino)-propionic Acid tert-Butyl Ester

trifluoroacetic acid

→

(2S)-2-(1-Adamantylmethoxycarbonylamino)-3-((5-(2-(1,4,5,6-tetrahydropyrimidin-2-ylcarbamoyl)-cyclopropyl)-thiophene-2-carbonyl)-amino)-propionic Acid

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvents were removed in vacuo
2. 2
   workup.DISSOLUTIONthe residue was dissolved in acetic acid
3. 3
   Sonstigethe solution was again evaporated to dryness
4. 4
   SonstigeThe resinous residue was triturated with diethyl ether
5. 5
   FiltrationAfter filtration 30 mg of the title compound
6. 6
   Sonstigewere obtained as a colourless amorphous powder

Vorschrift

48 mg of the product obtained in step c) were dissolved in 2 ml of dichloromethane and stirred for 3 hours with 1 ml of trifluoroacetic acid under an inert gas atmosphere at room temperature. The solvents were removed in vacuo, the residue was dissolved in acetic acid and the solution was again evaporated to dryness. This procedure was repeated once. The resinous residue was triturated with diethyl ether. After filtration 30 mg of the title compound were obtained as a colourless amorphous powder.

Quelle