反応 #155390

ord-ea6c47c487f949de97fe42aa0b7c794f

反応方程式

CN1c2ccccc2C(C(=O)O)c2ccccc21
10-methylacridan-9-carboxylic acid
CN1c2ccccc2C(C(=O)O)c2ccccc21
10-Methylacridan-9-carboxylic acid
O=S(Cl)Cl
thionyl chloride
Nc1ccc(N=Nc2ccc(S(=O)(=O)[O-])cc2)cc1S(=O)(=O)[O-].[Na+].[Na+]
yellow acid
CN1c2ccccc2C(C(=O)Cl)c2ccccc21
acid chloride
CN1c2ccccc2C(C(=O)Cl)c2ccccc21
10-Methylacridan-9-carboxylic acid chloride

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Into a 50 mL round bottom flask equipped with magnetic stirrer and under an argon atmosphere
  2. 2
    濃縮The light red brown solution was concentrated under reduced pressure
  3. 3
    その他the residue was dried for 15 min

実験手順

Into a 50 mL round bottom flask equipped with magnetic stirrer and under an argon atmosphere was charged a solution of 0.305 parts of 10-methylacridan-9-carboxylic acid (77) in 15 mL of dichloromethane and cooled to 5° C. (ice-water). Then, 1.05 parts of thionyl chloride was added to the cold yellow acid solution and stirred for 1.5 hr at a temperature below 15° C. The light red brown solution was concentrated under reduced pressure and the residue was dried for 15 min to give acid chloride (78).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08822233B2uspto-grants-2014_09