Реакция #3688

Уравнение реакции

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

2-dimethylaminoethanethiol hydrochloride

triethylamine

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

→

beige solid

Выход 93.1%

α-[[2-(Dimethylamino)ethyl]thio]-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]benzeneacetamide

Выход 93.1%

Растворители

methyl alcohol

Условия реакции

Обработка

1. 1
   ДругоеThe methyl alcohol 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 solid is dissolved in 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 to a residue which

Методика

A mixture of 0.14 g of α-chloro-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]benzeneacetamide, 0.47 g of 2-dimethylaminoethanethiol hydrochloride in 2 ml of methyl alcohol, 0.30 g of triethylamine and 3 ml of 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone is heated at 60° C. for 48 hours. The methyl alcohol is evaporated and the residue diluted with water. The resulting suspension is filtered and the precipitate washed with water. The solid is dissolved in ethyl acetate and washed with saturated NaHCO3, brine and dried with Na2SO4. The mixture is filtered and the filtrate evaporated in vacuo to a residue which is stirred with ether-hexane to give 0.15 g of beige solid. MS(CI): 525(M+H).

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