反応 #3603

反応方程式

10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

3-chlorobenzo[b]thiophen-2-carbonyl chloride

triethylamine

→

solid

収率 61.5%

N-[4-(5H-Pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]-3-chlorobenzo[b]thiophene-2-carboxamide

収率 61.5%

溶媒

methylene chloride

反応条件

後処理

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITcontinued for 18 hours
3. 3
   洗浄The reaction mixture is washed with water, 1N HCl, NaHCO3, and brine
4. 4
   乾燥The reaction mixture is dried with Na2SO4
5. 5
   ろ過filtered
6. 6
   その他evaporated in vacuo
7. 7
   その他to give a solid which
8. 8
   その他is purified by flash chromatography

実験手順

To a stirred solution of 0.440 g of 3-chlorobenzo[b]thiophen-2-carbonyl chloride in 10 ml of methylene chloride is added 0.33 ml of triethylamine. After stirring for 15 minutes, 0.485 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine is added and stirring continued for 18 hours. The reaction mixture is washed with water, 1N HCl, NaHCO3, and brine. The reaction mixture is dried with Na2SO4, filtered and evaporated in vacuo to give a solid which is purified by flash chromatography using 1:1 ethyl acetate-hexane to give 0.49 g of solid, m.p. 220°-222° C.

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