반응 #1869158

반응 방정식

5-amino-3-(2-dimethylaminoethyl)-1H-indol

5-chloro-3-methyl-benzo[b]thiophene-2-sulphonyl chloride

→

N-[3-(2-dimethylaminoethyl)-1H-indol-5-yl]-5-chloro-3-methyl-benzo[b]thiophene-2-sulphonamide

수율 82.0%

용매

pyridine

pyridine

반응 조건

후처리

1. 1
   기타It is then evaporated to dryness
2. 2
   workup.DISSOLUTIONdissolved in ethyl acetate
3. 3
   세척The organic phase is washed with water
4. 4
   기타a saturated solution of sodium bicarbonate, it is separated
5. 5
   건조dried with anhydrous sodium sulphate
6. 6
   기타The organic solution is evaporated to dryness
7. 7
   세척the resulting solid is repeatedly washed with ethyl ether

실험 절차

To a solution of 3.05 g (15 mMol) of 5-amino-3-(2-dimethylaminoethyl)-1H-indol in 100 ml of pyridine is added dropwise at ambient temperature a solution of 4.21 g (15 mMol) of 5-chloro-3-methyl-benzo[b]thiophene-2-sulphonyl chloride in 20 ml of pyridine. The reaction mixture is stirred at ambient temperature for 20 hours. It is then evaporated to dryness, slightly alkalinised with diluted ammonia and dissolved in ethyl acetate. The organic phase is washed with water and a saturated solution of sodium bicarbonate, it is separated and dried with anhydrous sodium sulphate. The organic solution is evaporated to dryness and the resulting solid is repeatedly washed with ethyl ether, to yield 5.5 g (82%) of N-[3-(2-dimethylaminoethyl)-1H-indol-5-yl]-5-chloro-3-methyl-benzo[b]thiophene-2-sulphonamide as a solid with m.p.=226-227° C.

출처