反応 #1137992

ord-c83431dbee6140ffa4cbfb6f6c76f336

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture was refluxed for 18 h
  2. 2
    ろ過was filtered
  3. 3
    濃縮The filtrate was concentrated in vacuo
  4. 4
    その他purified by flash chromatography on silica gel
  5. 5
    洗浄Eluting with 0-20% EtOAc/CH2Cl2

実験手順

To a solution of 7-(2,2-dimethyl-propionyloxy)-3-methyl-4-phenyl-isothiazolo[4,5-c]pyridine-6-carboxylic acid butyl ester (392 mg) in CCl4 (1.8 mL) was added N-bromosuccinimide (172 mg) and benzoyl peroxide (11.1 mg). The reaction mixture was refluxed for 18 h. After cooling to r.t. the mixture was filtered. The filtrate was concentrated in vacuo and purified by flash chromatography on silica gel. Eluting with 0-20% EtOAc/CH2Cl2 gave the title compound (398 mg) as a yellow oil: MS (m/z) 505.1 (M+1), 507.1 (M+1).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09387200B2uspto-grants-2016_07