Reaktion #43456

Reaktionsgleichung

4-(2-hydroxyethyl)-1,2-dihydro-3,6-pyridazinedione

triphenylphosphine

bis(1-methylethyl) (E)-1,2-diazenedicarboxylate

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product

Ausbeute 16.3%

5,6-Dihydrofuro[2,3-c]pyridazin-3(2H)-one

Ausbeute 16.3%

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter 3 hours the mixture was evaporated
2. 2
   Sonstigechromatographed onto silica which
3. 3
   workup.ADDITIONwas added to the top of a column
4. 4
   WaschenChromatography eluting with 0-10% methanol in DCM afforded impure product (420 mg) which
5. 5
   Sonstigewas further purified by chromatography in a similar manner

Vorschrift

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).

Quelle