反応 #1121703
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07893056B2
反応条件: temp:65.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of (3E)-2,2-dimethyl-1-(phenylcarbonyl)-3-pyrrolidinone O-methyloxime (1.9492 g, 7.914 mmol) in THF (80 mL) was added lithium aluminum hydride (0.900 g, 23.72 mmol), and the mixture was heated at 65° C. and stirred for 5 h. The mixture was cooled to 0° C., and Na2SO4.10H2O (2 g) was added. The mixture was stirred for 30 min, and 1 N aq. NaOH (100 mL) was then added. The mixture was extracted with Et2O (3×150 mL), and the combined organic phase was dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to give crude racemic 2,2-dimethyl-1-(phenylmethyl)-3-pyrrolidinamine (1.8247 g, >100% crude yield) as a light yellow oil. LCMS: (M+H)+: 205.2. The mixture was cooled to 0° C. The mixture was stirred for 30 min The mixture was extracted with Et2O (3×150 mL) the combined organic phase was dried over anhydrous Na2SO4 filtered concentrated in vacuo
ソース ID: ord-770b5be7e9c8469a9f710275435d62a3