Reaction #2027389

ord-47d32c717fcd4e328951d12ee3b810c4

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    TemperatureThe mixture was heated for 6 hours
  2. 2
    Temperatureunder reflux, to which
  3. 3
    FiltrationInsolubles were then filtered off
  4. 4
    ConcentrationThe filtrate was concentrated
  5. 5
    Otherwhich was purified by means of a silica gel column chromatography (hexane

Procedure

To tetrahydrofuran (20 ml) were added (3R,5S)-7-Chloro-5-(2-chlorophenyl)-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid (2 g) and aluminum lithium hydride (0.4 g). The mixture was heated for 6 hours under reflux, to which was added water. Insolubles were then filtered off. The filtrate was concentrated, which was purified by means of a silica gel column chromatography (hexane:acetic acid ethyl ester=2:1 v/v as an eluent) to give 1.65 g of non-crystalline solid matter.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05698691uspto-grants-1997_12