反応 #3688

反応方程式

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

収率 93.1%

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

収率 93.1%

溶媒

methyl alcohol

反応条件

後処理

1. 1
   その他The methyl alcohol is evaporated
2. 2
   workup.ADDITIONthe residue diluted with water
3. 3
   ろ過The resulting suspension is filtered
4. 4
   洗浄the precipitate washed with water
5. 5
   workup.DISSOLUTIONThe solid is dissolved in ethyl acetate
6. 6
   洗浄washed with saturated NaHCO3, brine
7. 7
   乾燥dried with Na2SO4
8. 8
   ろ過The mixture is filtered
9. 9
   その他the filtrate evaporated in vacuo to a residue which

実験手順

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).

出典