Reaktion #304084

ord-d85c8daa8e99494ea7e46176865567d7

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenconcentrated to ˜12 mL in vacuo
  2. 2
    workup.STIRRINGThe residue was stirred for 2 days
  3. 3
    workup.DISSOLUTIONdissolved in ethyl acetate/dichloromethane
  4. 4
    Waschenwashed with water containing an excess of sodium bicarbonate
  5. 5
    SonstigeThe organic layer was dried
  6. 6
    Sonstigeevaporated to the sub-titled compound (1.52 g)

Vorschrift

(S)-tert-Butyl 1-amino-3-(4-iodophenyl)-1-oxopropan-2-ylcarbamate (Example 1, step (i), 2.41 g) was stirred in dichloromethane (125 mL) and to the suspension was added trifluoroacetic acid (8 mL). The mixture was stirred for 2 h and then concentrated to ˜12 mL in vacuo. The residue was stirred for 2 days, dissolved in ethyl acetate/dichloromethane and washed with water containing an excess of sodium bicarbonate. The organic layer was dried and evaporated to the sub-titled compound (1.52 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08193239B2uspto-grants-2012_06