Aluminium lithium hydride → HCID 20193915, compound

Temperature

55 °C

Lithium aluminium hydride (475 mg, 12.49 mmol) was added portionwise to a stirred solution of 3-ethylperhydro-1,4-diazepin-2-one (740 mg, 5.20 mmol) in THF (10 mL). After the resultant effervescence had subsided, the reaction mixture was heated at 50-60° C. for 3 h. The reaction mixture was cooled and quenched by the slow addition of water and 10% NaOH (aq.). The reaction mixture was diluted with diethyl ether (20 mL) and filtered through celite. The filter cake was washed thoroughly with THF (50 mL), diethyl ether (50 mL), THF (50 mL) and diethyl ether (50 mL). Evaporation under reduced pressure afforded 2-ethylperhydro-1,4-diazepine (INTERMEDIATE X.1) (615 mg, 5.20 mmol), 92%).

1. temperatureThe reaction mixture was cooled
2. customquenched by the slow addition of water and 10% NaOH (aq.)
3. additionThe reaction mixture was diluted with diethyl ether (20 mL)
4. filtrationfiltered through celite
5. washThe filter cake was washed thoroughly with THF (50 mL), diethyl ether (50 mL), THF (50 mL) and diethyl ether (50 mL)
6. customEvaporation under reduced pressure

ORD record

ord-2b4a8e7d03a94c4daba2a3904532638a

Source dataset

uspto-grants-2010_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07820649B2