反应详情

温度

125 °C

To 14 g (0.14 mol) of 3-amino-N-methyl pyrroline was added 10.4 g (0.042 mol) of N-benzyl-2-chlorobenzimidazole and the reaction mixture heated to 125° C. for 2 days. The reaction mixture was partitioned between 150 mL of 1N NaOH and 100 mL of CH2Cl2. The aqueous layer was extracted again with 100 mL of CH2Cl2. The combined organic layers were washed with 100 mL of 1N NaOH, dried over Na2SO4, filtered, and concentrated by rotary evaporation and subjected to high vacuum at 100° C. for ~30 min. For purification, the residue was treated with 2 moles of oxalic acid in ethanol/2-propanol to afford 15 g (73%) of white analytically pure crystals, mp 211°-213° C. dec.

1. customThe reaction mixture was partitioned between 150 mL of 1N NaOH and 100 mL of CH2Cl2
2. extractionThe aqueous layer was extracted again with 100 mL of CH2Cl2
3. washThe combined organic layers were washed with 100 mL of 1N NaOH
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated by rotary evaporation
7. waitsubjected to high vacuum at 100° C. for ~30 min
8. customFor purification
9. customto afford 15 g (73%) of white analytically pure crystals, mp 211°-213° C. dec.