Reaktion #3693

Reaktionsgleichung

2-chloro-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]acetamide

morpholine

1,3-di-methyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone

→

colorless gum

Ausbeute 106.8%

N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]-4-morpholineacetamide

Ausbeute 106.8%

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe methylene chloride is evaporated
2. 2
   workup.ADDITIONthe residue diluted with water
3. 3
   FiltrationThe resulting suspension is filtered
4. 4
   Waschenthe precipitate washed with water
5. 5
   workup.DISSOLUTIONThe brown solid is dissolved in 15 ml of ethyl acetate
6. 6
   Waschenwashed with saturated NaHCO3, brine
7. 7
   Trocknendried with Na2SO4
8. 8
   FiltrationThe mixture is filtered
9. 9
   Sonstigethe filtrate evaporated in vacuo

Vorschrift

A stirred suspension of 0.19 g of 2-chloro-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]acetamide in 1 ml of methylene chloride is added 0.44 g of morpholine followed by 1 ml of 1,3-di-methyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone and stirring continued for 20 hours. The methylene chloride is evaporated and the residue diluted with water. The resulting suspension is filtered and the precipitate washed with water. The brown solid is dissolved in 15 ml of ethyl acetate and washed with saturated NaHCO3, brine and dried with Na2SO4. The mixture is filtered and the filtrate evaporated in vacuo to give 0.23 g of a colorless gum which is stirred with ethyl acetate-hexanes to give 0.21 g of white solid. MS(CI): 431(M+H).

Quelle