Reaktion #2288465

ord-b7914579137647ccbd229a2073c6481e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigereaction
  2. 2
    Extraktionextracted with DCM (3×20 ml) The
  3. 3
    Einengenconcentrated in vacuo
  4. 4
    Sonstigeto yield a yellow oil
  5. 5
    SonstigeThe material was used without further purification

Vorschrift

To a solution of (R)-6-(2-hydroxypropyl)-1,3-dimethyl-5-phenyl-1H-pyrrolo[3,4-d]pyrimidine-2,4(3H,6H)-dione (step 1) (925 mg, 2.95 mmol) in DCE (16 ml) was added triethylamine (2.05 ml, 14.8 mmol), DMAP (36 mg, 0.29 mmol) and methanesulfonyl chloride (1.15 ml, 14.8 mmol) at 0° C. and reaction stirred for 30 min. Solid K2CO3 was added to the reaction mixture and the resulting mixture was diluted with water and extracted with DCM (3×20 ml) The organics were passed through a hydrophobic frit and concentrated in vacuo to yield a yellow oil. The material was used without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09359381B2uspto-grants-2016_06