反应详情

温度

0 °C

A suspension of 11.5 g. (50 mMol) ethyl 4-(2-aminoethyl)-benzoate hydrochloride (J.A.C.S., 65, 2281, 2284/1943) and 12.65 g. (125 mMol) triethylamine in 150 ml. methylene chloride is stirred for 30 minutes at ambient temperature, cooled to 0° C. and a solution of 11.55 g. (50 mMol) 4-chlorobenzenesulphonic acid chloride in 50 ml. methylene chloride slowly added dropwise thereto. After ending of the reaction, the reaction mixture is extracted twice with dilute hydrochloric acid, washed with water and the organic phase then dried over anhydrous sodium sulphate. After evaporation of the solvent, there are obtained 11.4 g. (62% of theory) of colourless crystals; m.p. 88° C., after recrystallisation from ethanol.

1. additionA suspension of 11.5 g
2. customAfter ending of the reaction
3. extractionthe reaction mixture is extracted twice with dilute hydrochloric acid
4. washwashed with water
5. dry with materialthe organic phase then dried over anhydrous sodium sulphate
6. customAfter evaporation of the solvent, there
7. customare obtained 11.4 g
8. customm.p. 88° C., after recrystallisation from ethanol