反応 #3175

ord-2d4f64dd7b0a4a1ab9ebcd6c62f6820c

反応方程式

O=C(O)CCC(=O)c1ccc(C(=O)C2(O)CCCCC2)cc1
1-hydroxycyclohexyl 4-(2-carboxyethyl)carbonylphenyl ketone
O=S(Cl)Cl
thionyl chloride
O=C(Cl)CCC(=O)c1ccc(C(=O)C2(O)CCCCC2)cc1
1-hydroxycyclohexyl 4-(2-chloroformylethyl)carbonylphenyl ketone
収率 94.0%

反応条件

温度
30°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他A 250-ml round-bottomed flask fitted with a condenser
  2. 2
    その他The resulting reaction mixture
  3. 3
    その他after which time the solvent was removed under reduced pressure
  4. 4
    温度The residue, a white solid, was maintained at 0.01 Torr =30 minutes
  5. 5
    その他to remove residual solvent and excess thionyl chloride

実験手順

A 250-ml round-bottomed flask fitted with a condenser was charged with 12.0 g of 1-hydroxycyclohexyl 4-(2-carboxyethyl)carbonylphenyl ketone (0.04 mole), 5.95 g (0.05 mole) of thionyl chloride (Aldrich), and 50 ml of diethyl ether. The resulting reaction mixture was stirred at 30° C. for 30 minutes, after which time the solvent was removed under reduced pressure. The residue, a white solid, was maintained at 0.01 Torr =30 minutes to remove residual solvent and excess thionyl chloride, leaving 12.1 g (94 percent) of 1-hydroxycyclohexyl 4-(2-chloroformylethyl)carbonylphenyl ketone.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05733693uspto-grants-1998_03