反应详情

A mixture of 2-(1-methyl-cyclopropyl)-pyran-4-one (Step 1.6) (66.6 mmol) and a 28-30% aqueous solution of ammonium hydroxide (182 mL) was stirred for 1 h at 65° C. After cooling to rt, the reaction mixture was decanted to remove a dark brown solid and then concentrated. The residue was diluted with MeOH and re-concentrated (3×) to afford the title compound as a brown-orange solid. HPLC: tR=3.56 min (method B); LC-MS: tR=0.87 min, [M+H]+ 151; TLC: Rf=0.18 (9:1 CH2Cl2/MeOH).

1. customthe reaction mixture was decanted
2. customto remove a dark brown solid
3. concentrationconcentrated
4. additionThe residue was diluted with MeOH
5. concentrationre-concentrated (3×)