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 equipped 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-5913679be0b645d4b04950eb87fde42b

Source dataset

uspto-grants-2012_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08242153B2