Reaktion #44404

ord-ae6c6ebfed9b49a7974c79fca2e657ca

Lösungsmittel

Reaktionsbedingungen

Temperatur
65°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe mixture was filtered by vacuum filtration
  2. 2
    SonstigeThe filtrate was collected
  3. 3
    workup.STIRRINGwhile stirring
  4. 4
    FiltrationThe resulting precipitate was collected by vacuum filtration

Vorschrift

Crude MTC product (MW 373.90, 10.0 g, ˜26.7 mmol) was fully dissolved in H2O (270 cm3). Ethylenediaminetetraacetic acid (EDTA) disodium salt dihydrate (MW 372.24, 1 g, 2.68 mmol, 0.1 equivalents) was added. The mixture was stirred at 65° C. for approximately 1 hour. The mixture was filtered by vacuum filtration. The filtrate was collected. Sodium chloride (NaCl, MW 57.96, 16 g, 0.276 mol, 10 equivalents) was added to the filtrate while stirring. The resulting precipitate was collected by vacuum filtration.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07737138B2uspto-grants-2010_06