反应详情

6-(4-Chlorophenyl)-7-phenyl-2,3-dihydro-1H-pyrrolizine (Example 17 a, 1.5 g, 5.1 mmol), dissolved in THF (10 ml), is treated with 1 drop of triethylamine (about 50 mg). A solution of diphosgene (0.5 g, 2.5 mmol), dissolved in THF (5 ml), is added dropwise to this solution at RT and it is stirred for 8 h. Methanol (abs., 3 ml) is then added, and the mixture is stirred at RT for a further 12 h. The solvent is completely removed in vacuo (45° C.). The resinous residue is dissolved in CHCl3 (20 ml) and washed twice with water (20 ml). After the removal of the solvent in vacuo, a residue which is recrystallized from a little diisopropyl ether is obtained from the CHCl3 phase dried using Na2SO4 sicc.

1. additionis added dropwise to this solution at RT
2. stirringthe mixture is stirred at RT for a further 12 h
3. customThe solvent is completely removed in vacuo (45° C.)
4. dissolutionThe resinous residue is dissolved in CHCl3 (20 ml)
5. washwashed twice with water (20 ml)
6. customAfter the removal of the solvent in vacuo
7. customa residue which is recrystallized from a little diisopropyl ether
8. customis obtained from the CHCl3 phase
9. customdried