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0 °C

A suspension of methyl (3,6-dioxo-1,2,3,6-tetrahydro-4-pyridazinyl)acetate (11.1 g, 60.3 mmol) in THF (2 litres) was sonicated to give a fine dispersion. The mixture was called to −15° C. and treated dropwise with a solution of lithium aluminium hydride in THF (1M; 90 ml, 90 mmol). The mixture was stirred at 0° C. for 2 hours. Sodium hydroxide (2M; 15 ml, 30 mmol) was added, then the mixture was acidified with 5M hydrochloric acid to around pH4-5. The supernatant was decanted off and discarded. The oily residue was extracted with water/methanol (500 ml/1 litre). This extract was decanted from the remaining residue, treated with silica and evaporated. The silica residue was added to the top of a column, eluting with 10-30% methanol in DCM affording a pale yellow oil (2.7 g).

1. customwas sonicated
2. customto give a fine dispersion
3. customwas called to −15° C.
4. customThe supernatant was decanted off
5. extractionThe oily residue was extracted with water/methanol (500 ml/1 litre)
6. customThis extract was decanted from the remaining residue
7. additiontreated with silica
8. customevaporated
9. additionThe silica residue was added to the top of a column
10. washeluting with 10-30% methanol in DCM affording a pale yellow oil (2.7 g)