反応 #1869158

反応方程式

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

収率 82.0%

溶媒

pyridine

pyridine

反応条件

後処理

1. 1
   その他It is then evaporated to dryness
2. 2
   workup.DISSOLUTIONdissolved in ethyl acetate
3. 3
   洗浄The organic phase is washed with water
4. 4
   その他a saturated solution of sodium bicarbonate, it is separated
5. 5
   乾燥dried with anhydrous sodium sulphate
6. 6
   その他The organic solution is evaporated to dryness
7. 7
   洗浄the resulting solid is repeatedly washed with ethyl ether

実験手順

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.

出典