反应详情

With gentle heating, 22a (1.5 g; 5.4 mmol) was dissolved in methanol (15 ml). The solution was cooled to room temperature, HCl-containing methanol (20 ml) was added and the mixture was transferred into a two-necked flask. Pd—C 10% (150 mg) was introduced into the initial charge. The reaction vessel was evacuated using an oil pump, and H2 was then introduced via a gas inlet capillary (4×). At room temperature, the suspension was shaken in a closed three-necked flask under an atmosphere of H2 (240 strokes/min) until no more starting material could be detected by thin-layer chromatography (6 h). The suspension was filtered and the catalyst was washed with plenty of methanol. The combined filtrate was concentrated and the mustard-colored solid-amorphous residue was dried using an oil pump. The crude product was used without further purification for the next reaction step.

1. additionwas added
2. customthe mixture was transferred into a two-necked flask
3. additioninitial charge
4. customThe reaction vessel was evacuated
5. additionwas then introduced via a gas inlet capillary (4×)
6. customcould be detected by thin-layer chromatography (6 h)
7. filtrationThe suspension was filtered
8. washthe catalyst was washed with plenty of methanol
9. concentrationThe combined filtrate was concentrated
10. customthe mustard-colored solid-amorphous residue was dried
11. customThe crude product was used without further purification for the next reaction step