反応 #58601

ord-c4081059b5ec48d99cfec68090949e81

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGstirring
  2. 2
    workup.WAITcontinues for 15 minutes
  3. 3
    その他the layers are separated

実験手順

A solution of dimethylsulphoxide (0.69 mL, 9.7 mmol, 2.2 eq) in DCM (4.5 mL) is slowly added to a solution of oxalyl chloride (2.43 mL, 4.85 mmol, 1.1 eq) in DCM (2.5 mL) followed by a solution of 76 (1.09 g, 4.41 mmol) in DCM (0.7 mL) under nitrogen at −60° C. After stirring for 15 minutes, triethylamine (3.14 mL, 22.1 mmol, 5 eq) is added and stirring continues for 15 minutes. After addition of water, the layers are separated.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07423037B2uspto-grants-2008_09