反应详情

A mixture containing 4-methoxyphenyl hydrazine . HCl (70.66 g, 0.405 mol) and methyl 5-(t-butylthio)-2,2-dimethyl-4-oxopentanoate (99.54 g, 0.405 mol) in tBuOH (400 ml) was heated at a gentle reflux for 48 hours. The mixture was allowed to cool to RT and the precipitated NH4Cl was removed by filtration. The residue was concentrated and fractionated on a plug of silica using EtOAc/hexane (1:3) as eluent. Evaporation of the appropriate fraction gave an orange-brown solid which was crystallized from EtOH (100 ml). Yield from two crops afforded 55.6g of the title compound.

1. temperaturewas heated at
2. temperaturea gentle reflux for 48 hours
3. customthe precipitated NH4Cl was removed by filtration
4. concentrationThe residue was concentrated
5. customEvaporation of the appropriate fraction
6. customgave an orange-brown solid which
7. customwas crystallized from EtOH (100 ml)
8. customYield from two crops