反应详情

To a solution of N-(cholest-5-en-3β-oxycarbonyl)glycine (160.8 mg) in dry tetrahydrofuran (50 ml) was added said bis(2-chloroethyl)amine (85.2 mg) and dicyclohexylcarbodiimide (61.9 mg) at 0° C. under blowing nitrogen gas and the mixture was stirred for 6 hours. After standing overnight (17 hours) at refrigerator, the reaction mixture was filtered and the solvent was evaporated under reduced pressure. The residue was solved in a mixture of chloroform and methanol (50:1) and was subjected to preparation column chromatography (PLC) eluting with a mixture of chloroform and methanol (50:1). The desired parts were gathered, extracted with a mixture of chloroform and methanol (4:1), filtered and concentrated under reduced pressure to give N-[N-(cholest-5-en-3β-oxycarbonyl)glycyl]bis(2-chloroethyl)amine (110 mg).

1. customat 0° C.
2. waitAfter standing overnight
3. filtration(17 hours) at refrigerator, the reaction mixture was filtered
4. customthe solvent was evaporated under reduced pressure
5. additionThe residue was solved in a mixture of chloroform and methanol (50:1)
6. customwas subjected to preparation column chromatography (PLC)
7. washeluting with a mixture of chloroform and methanol (50:1)
8. extractionextracted with a mixture of chloroform and methanol (4:1)
9. filtrationfiltered
10. concentrationconcentrated under reduced pressure