Hydrochloric Acid → HCID 67177917, compound

Temperature

60 °C

To a stirred suspension of 3,3-dimethyl-4-phenyl-butyraldehyde (2.46 g; CAS 15674-36-9) at r.t. in ethanol (25 ml) under an argon atmosphere were added H2O (25 ml), ammonium carbonate (6.71 g) and NaCN (0.82 g). The mixture was heated to 60° C. (internal temperature), and stirring was continued for 17 h. The mixture was cooled to 0° C. The reactor was equiped with a 4 N NaOH trap in order to trap the evolving HCN. 3 N HCl (25 ml) was added dropwise for 10 min (temperature of the reaction mixture not over 9° C. during the addition). When addition was complete, a stream of air was passed through the reaction mixture (still kept in an ice bath) for 30 min in order to ensure complete removal of HCN. The product was collected by filtration, washed with plenty of H2O and cyclohexane and dried to give (RS)-5-(2,2-dimethyl-3-phenyl-propyl)-imidazolidine-2,4-dione (2.05 g) as off-white powder. MS (ISN): 245.2 ([M−H]−))

1. temperatureThe mixture was cooled to 0° C
2. additionduring the addition)
3. additionWhen addition
4. customstill kept in an ice bath
5. wait) for 30 min in order to ensure complete
6. customremoval of HCN
7. filtrationThe product was collected by filtration
8. washwashed with plenty of H2O and cyclohexane
9. customdried

ORD record

ord-1c2a4896f5b94583863a940683ac936b

Source dataset

uspto-grants-2014_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08729113B2