反应详情

To a solution of #5 (26 g, 42 mmol, 1 eq.) in tetrahydrofuran (260 mL, 0.16 M) was added diethylamine (22 mL) over 30 minutes. The reaction was stirred for about 6 hours and the suspension was then filtered through Celite and washed with additional tetrahydrofuran (25 mL). The filtrate was concentrated in vacuo to provide a pale yellow oil, which was redissolved in 2-methyltetrahydrofuran (50 mL) and concentrated again to ensure complete removal of diethylamine. The crude oil of #6 (>15.25 g) was taken into the next step without further purification.

1. filtrationthe suspension was then filtered through Celite
2. washwashed with additional tetrahydrofuran (25 mL)
3. concentrationThe filtrate was concentrated in vacuo
4. customto provide a pale yellow oil, which
5. concentrationconcentrated again
6. customremoval of diethylamine
7. customThe crude oil of #6 (>15.25 g) was taken into the next step without further purification