反応 #3370675
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06630461B2
反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 4-(t-butoxycarbonylamino)-benzeneacetic acid (2.9 g, 11.4 mmoles) is dissolved in 10 ml of anhydrous THF at 0° C. and added to a suspension of LiAlH4 (0.52 g, 13.6 mmoles) in 30 ml of THF. The reaction mixture is agitated at ambient temperature for 1.5 hours. 50 ml of ethyl acetate then 20 ml of 2N soda are added to the medium. The expected product is extracted from the organic phase, which is then washed with 3 times 15 ml of water. The organic phase is dried and the solvent evaporated off under reduced pressure. Then the reaction product is purified on silica gel in a dichloromethane/methanol mixture (95/5). 1.1 g (40%) is thus obtained in the form of a colourless oil. The expected product is extracted from the organic phase, which is then washed with 3 times 15 ml of water The organic phase is dried the solvent evaporated off under reduced pressure Then the reaction product is purified on silica gel in a dichloromethane/methanol mixture (95/5) 1.1 g (40%) is thus obtained in the form of a colourless oil
ソース ID: ord-246dd5c7e2a94ad090201608be540e52