Oxygen → 2-Butyl-5-formylimidazole

4.6 g of 2-n-butyl-5-hydroxymethylimidazole, 4.6 g of dodecane as internal GC standard, 0.6 g of 5 percent platinum and 5 percent bismuth on activated carbon (comprising 61.3 percent water), 42 g of isobutyl methyl ketone and 7.5 g of 1.6 percent strength NaOH solution were heated to about 80° C. with stirring. At 80° C., 3.6 liters (STP) of air/hour was introduced into the solution until the absorption of oxygen was complete (350 min!). The reaction mixture was filtered. The filtrate was transferred to a separating funnel, the H2O phase was separated off, the organic phase was concentrated and cooled, and the product crystallized out and was filtered off. The reaction was monitored using GC analysis (internal standard). The reaction yield was 90.0 percent (0.3 percent of starting material).

1. custom(350 min!)
2. filtrationThe reaction mixture was filtered
3. customThe filtrate was transferred to a separating funnel
4. customthe H2O phase was separated off
5. concentrationthe organic phase was concentrated
6. temperaturecooled
7. customthe product crystallized out
8. filtrationwas filtered off
9. customThe reaction yield was 90.0 percent (0.3 percent of starting material)

ORD record

ord-349acd7c3f5c473487fe745114cabc20

Source dataset

uspto-grants-2000_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06040457