반응 #155401
ord-1ec9bc3d671e44158047973099138a77
반응 방정식
N-Fmoc-4-amino-butyraldehyde diethyl acetal
HCl
→
N-Fmoc-4-amino-butyraldehyde
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타Upon completion, the organic solvent was removed by rotary evaporation
- 2추출the aqueous layer was extracted with ethyl acetate (2×200 mL)
- 3세척The combined organic layers were washed with 5% NaHCO3 (2×75 mL), brine (75 mL)
- 4건조dried over Na2SO4
- 5여과filtered
- 6농축concentrated to dryness
실험 절차
To a stirring solution of N-Fmoc-4-amino-butyraldehyde diethyl acetal (0.050 mmol) in 1,4-dioxane (100 mL) was added aq. HCl (100 ml, 1:1 v/v, H2O:conc. HCl) and the reaction progress was monitored by MS. Upon completion, the organic solvent was removed by rotary evaporation, and the aqueous layer was extracted with ethyl acetate (2×200 mL). The combined organic layers were washed with 5% NaHCO3 (2×75 mL), brine (75 mL), dried over Na2SO4, filtered and concentrated to dryness to yield the desired N-Fmoc-4-amino-butyraldehyde (15.35 g, 0.049 mol, 90.0% yield), which was carried through to the next step without further purification: MS m/e [M+Na]+ calcd 332.1. found 332.0.