Hydrochloric Acid → HCID 59707067, compound

Sodium hydride (approximately 60% strength suspension in oil, 1.2 g, approximately 30 mmol) was added portionwise to a solution of imidazolidin-2-one (2.58 g, 30 mmol) in abs. DMF (40 mL) under a blanket of argon within 10 min. The reaction mixture was stirred for 90 min at RT and a solution of 4-tert-butylbenzyl bromide (3.7 mL, 20.1 mmol) in abs. DMF (3 mL) was then added. The reaction mixture was stirred at RT over a period of 3 h and then added to a mixture of H2O (100 mL) and 2N hydrochloric acid solution in H2O (10 mL). The resulting mixture was stirred for 30 min, and the resulting crystals were separated with the aid of a frit and washed with H2O (3×30 mL). The isolated solid matter was recrystallized from a mixture of H2O (100 mL) and EtOH (120 mL). The substance formed (1.4 g, mp: 122-127° C.) is compound D.

1. stirringThe reaction mixture was stirred at RT over a period of 3 h
2. stirringThe resulting mixture was stirred for 30 min
3. customthe resulting crystals were separated with the aid of a frit
4. washwashed with H2O (3×30 mL)
5. customThe isolated solid matter was recrystallized from a mixture of H2O (100 mL) and EtOH (120 mL)
6. customThe substance formed (1.4 g, mp: 122-127° C.)

ORD record

ord-eb5e6b7f50f84665aa1553316c73ed99

Source dataset

uspto-grants-2012_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08207182B2