反应详情

A solution of 1.82 ml. diethanolamine (2 g., 0.0189 mole) in 10 ml. of tetrahydrofuran is added to a mixture of N-[3-(mercaptoacetylamino)benzoyl]glycine (5 g., 0.0186 mole), 5 mg. of disodium edetate, 4 ml. of water and 40 ml. of tetrahydrofuran under an atmosphere of nitrogen during a 5-minute period at room temperature. The resulting mixture is first warmed to 40°-45° C. for 20 min. and then cooled in a dry ice-ethanol bath for 0.5 hr. to promote crystallization. Cooling is discontinued and the mixture stirred overnight under an atmosphere of nitrogen and filtered. The material collected is washed with tetrahydrofuran and then dried under vacuum over calcium chloride to provide 5.8 g., of the bis-(2-hydroxyethyl) ammonium salt of N-[3 -(mercaptoacetylamino)benzoyl]glycine, m.p. 64°-74.5° C. (dec.).

1. temperatureThe resulting mixture is first warmed to 40°-45° C. for 20 min.
2. temperaturecooled in a dry ice-ethanol bath for 0.5 hr
3. customcrystallization
4. temperatureCooling
5. filtrationfiltered
6. customThe material collected
7. washis washed with tetrahydrofuran
8. dry with materialdried under vacuum over calcium chloride
9. customto provide 5.8 g