反应详情

2-((6-chrysenylmethyl)amino)-2-methyl-1,3-propanediol methanesulfonate (1C, 10.0 g, 26.63 mmol) was neutralized with 1N NaOH (30 mL) in CH3OH/H2O (200/800 mL) as in procedure 1D. The white solid which formed was filtered, washed successively with warm H2O (3×500 mL), CH3OH (200 mL), and abs. Et2O (2×500 mL), sucked semi-dry and then resuspended in CH3OH (500 mL). To this was added a 0.43M aqueous solution of 2-hydroxyethanesulfonic acid (30 mL). Slight warming gave a solution which was then filtered. The solvent was removed by rotary evaporation to give a wet white solid. This was triturated with dry Et2O, filtered, and recrystallized 3× from EtOH/Et2O to give 8.8 g (70.4%) of 2-((6-chrysenylmethyl)amino)-2-methyl-1,3-propanediol 2-hydroxyethanesulfonate, mp 212°-213°, (C, H, N, S).

1. customThe white solid which formed
2. filtrationwas filtered
3. washwashed successively with warm H2O (3×500 mL), CH3OH (200 mL), and abs
4. additionTo this was added a 0.43M aqueous solution of 2-hydroxyethanesulfonic acid (30 mL)
5. temperatureSlight warming
6. customgave a solution which
7. filtrationwas then filtered
8. customThe solvent was removed by rotary evaporation
9. customto give a wet white solid
10. customThis was triturated with dry Et2O
11. filtrationfiltered
12. customrecrystallized 3× from EtOH/Et2O