反应 #452449

ord-36f903ae0afc4ed6b419143fa000bc71

反应方程式

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
收率 94.0%

反应条件

温度
30°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他A 250-ml round-bottomed flask fitted with a condenser
  2. 2
    其他The resulting reaction mixture
  3. 3
    其他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 for 30 minutes
  5. 5
    其他to remove residual solvent and excess thionyl chloride

实验过程

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 Chemical Co., Milwaukee, Wis.), 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 for 30 minutes to remove residual solvent and excess thionyl chloride, leaving 12.1 g (94 percent) of 1-hydroxycyclohexyl 4-(2-chloroformylethyl)carbonylphenyl ketone.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06127073uspto-grants-2000_10