Реакция #3693

Уравнение реакции

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

Выход 106.8%

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

Выход 106.8%

Растворители

methylene chloride

Условия реакции

Обработка

1. 1
   ДругоеThe methylene chloride is evaporated
2. 2
   workup.ADDITIONthe residue diluted with water
3. 3
   ФильтрацияThe resulting suspension is filtered
4. 4
   Промывкаthe precipitate washed with water
5. 5
   workup.DISSOLUTIONThe brown solid is dissolved in 15 ml of ethyl acetate
6. 6
   Промывкаwashed with saturated NaHCO3, brine
7. 7
   Сушкаdried with Na2SO4
8. 8
   ФильтрацияThe mixture is filtered
9. 9
   Другоеthe filtrate evaporated in vacuo

Методика

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).

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