Octahydro-2H-azonin-2-one → HCID 23665043, compound

Temperature

110 °C

A 5 L three-neck round bottom flask was fitted with a heating mantle, an overhead mechanical stirrer, a reflux condenser, and a thermometer. A suspension of 2-azacyclononanone (83 g, 0.59 moles, 1.0 equiv.) in 5 M aqueous sodium hydroxide (650 mL, 3.23 moles, 5.5 equiv.) was charged into the round bottom flask. The mixture was heated to reflux (internal temperature about 110° C.) for 4 hours to yield a clear yellow solution. The heating mantle and reflux condenser were removed. After the solution cooled to room temperature, it was diluted with water (650 mL) and cooled further in an ice bath.

1. customA 5 L three-neck round bottom flask was fitted with a heating mantle, an overhead mechanical stirrer, a reflux condenser
2. additionwas charged into the round bottom flask
3. temperatureThe mixture was heated
4. customto yield a clear yellow solution
5. temperatureThe heating mantle and reflux condenser
6. customwere removed
7. temperatureAfter the solution cooled to room temperature
8. additionit was diluted with water (650 mL)
9. temperaturecooled further in an ice bath

ORD record

ord-59c2782f17c741f6bd58cb99407ffc4b

Source dataset

uspto-grants-2000_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06084112