反应详情

A solution 1.13 ml. of ethanolamine (1.15 g., 0.0188 mole) and 10 ml. of tetrahydrofuran is added to a suspension of N-[3-(mercaptoacetylamino)benzoyl]glycine (5 g., 0.0186 mole), 5 mg. of disodium edetate, 6 ml. of water, and 40 ml. of tetrahydrofuran. Warming the mixture to 40°-45° C. provides a clear solution which is first diluted with 200 ml. of tetrahydrofuran, then cooled in a dry ice-acetone bath to promote crystallization and subsequently stirring for a period of 16 hrs. at room temperature. The precipitated material formed is collected, washed with tetrahydrofuran and dried over calcium chloride to afford 5.7 g., (93% yield) of N-[3-(mercaptoacetylamino)benzoyl]glycine 2-hydroxyethyl ammonium salt, m.p. 144.0°-160.0° C. (dec.).

1. temperatureWarming the mixture to 40°-45° C.
2. customprovides a clear solution which
3. additionis first diluted with 200 ml
4. customcrystallization
5. customat room temperature
6. customThe precipitated material formed
7. customis collected
8. washwashed with tetrahydrofuran
9. dry with materialdried over calcium chloride
10. customto afford 5.7 g