反応 #2460302

ord-687f2cd48e64426183354893f175f10f

反応方程式

O=C(O)c1ccc2sc3ccccc3c(=O)c2c1
Thioxanthen-9-one-2-carboxylic acid
CCCO
n-propanol
O=S(=O)(O)O
sulfuric acid
CCCOC(=O)c1ccc2sc3ccccc3c(=O)c2c1
propyl thioxanthen-9-one-2-carboxylate

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度heated
  2. 2
    温度at reflux
  3. 3
    濃縮The reaction mixture was concentrated
  4. 4
    洗浄the resulting solid residue was washed with water
  5. 5
    その他dried
  6. 6
    その他The product was purified by recrystallization from heptane
  7. 7
    その他to provide 26.6 g (65% of theory) of a pale yellow solid

実験手順

Finally, propyl thioxanthen-9-one-2-carboxylate (S-20) was prepared. Thioxanthen-9-one-2-carboxylic acid (35 g, 137 mmol) was suspended in a mixture of toluene (250 mL), n-propanol (250 mL), and concentrated sulfuric acid (2 mL) and heated at reflux with stirring for 3 d. The reaction mixture was concentrated, and the resulting solid residue was washed with water and dried. The product was purified by recrystallization from heptane to provide 26.6 g (65% of theory) of a pale yellow solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07459263B2uspto-grants-2008_12