反应详情

温度

40 °C

A mixture of 4-(2-hydroxyethyl)-1,2-dihydro-3,6-pyridazinedione (2.7 g) in THF (200 ml) was treated with triphenylphosphine (6.6 g) and bis(1-methylethyl) (E)-1,2-diazenedicarboxylate (5.0 ml) was warmed to 40° C. After 3 hours the mixture was evaporated and chromatographed onto silica which was added to the top of a column. Chromatography eluting with 0-10% methanol in DCM afforded impure product (420 mg) which was further purified by chromatography in a similar manner affording the product (390 mg).

1. customAfter 3 hours the mixture was evaporated
2. customchromatographed onto silica which
3. additionwas added to the top of a column
4. washChromatography eluting with 0-10% methanol in DCM afforded impure product (420 mg) which
5. customwas further purified by chromatography in a similar manner