反应详情

温度

0 °C

Trifluoroacetic acid (25 mL) was slowly dripped into a solution of (4) (7.10 g, 13.93 mmol) in CH2Cl2 (150 mL) which had been cooled to 0° C. The solution was stirred at 0° C. for 30 minutes and at room temperature for 15 minutes. Solvent and excess TFA were removed by rotary evaporation, and the concentrate was cooled to 0° C., treated with saturated NaHCO3 (150 mL) and extracted with CH2Cl2 (4×80 mL). After solvent removal, the crude oil was purified by silica gel column chromatography with 1:1 hexane/EtOAc as the eluant, generating 4.6 g (81%) of (5) as an oil: NMR δ 1.40-190 (m, 8H), 2.30 (t, 2H, J=6), 2.40 (t, 2H, J=6), 2.90 (t, 2H, J=6), 3.63 (t, 2H, J= 6), 4.63 (s, 2H), 4.75 (s, 2H), 4.93 (br s, 1H), 7.27 (s, 5H), 7.33 (s, 5H). Anal. (C24H31N3O3) C, H, N.

1. customSolvent and excess TFA were removed by rotary evaporation
2. temperaturethe concentrate was cooled to 0° C.
3. additiontreated with saturated NaHCO3 (150 mL)
4. extractionextracted with CH2Cl2 (4×80 mL)
5. customAfter solvent removal
6. customthe crude oil was purified by silica gel column chromatography with 1:1 hexane/EtOAc as the eluant