反应详情

Dichlorodicyanoquinone (340.8 g, 1,500 mmol) was added to a stirred solution of the title compound of Example 4 (361.4 g, 681 mmol) dissolved in tetrahydrofuran (15 L) and heated to reflux for 6 hours at which time HPLC indicated complete reaction. The reaction was concentrated to ¼ its volume and diluted with ethyl acetate (12 L). The resulting black solution was washed three times with saturated aqueous NaHCO3 (5.5 L). The organic layer was dried over sodium sulfate and concentrated to give the title compound as a black solid (392 g, 100% yield). 1H NMR (CDCl3): consistent with proposed structure.

1. temperatureheated
2. temperatureto reflux for 6 hours at which time HPLC
3. customreaction
4. concentrationThe reaction was concentrated
5. additiondiluted with ethyl acetate (12 L)
6. washThe resulting black solution was washed three times with saturated aqueous NaHCO3 (5.5 L)
7. dry with materialThe organic layer was dried over sodium sulfate
8. concentrationconcentrated