反应 #1994243

ord-d6d60343bd5e4faba8cf8df11ffe0555

反应方程式

CC(=O)C1CCC(=O)N1C(C)=O
Compound 5
CC(=O)C1CCC(=O)N1C(C)=O
N,5-diacetylpyrrolidin-2-one
O=C([O-])[O-].[K+].[K+]
K2CO3
Cl
hydrochloric acid
CC(=O)C1CCC(=O)N1
Compound 6
收率 48.0%
CC(=O)C1CCC(=O)N1
5-acetylpyrrolidin-2-one
收率 48.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGAfter stirring for 3.5 hrs
  2. 2
    其他freeze-dried for 16 hrs
  3. 3
    萃取The organic residue is then extracted with CH2Cl2 (40 mL)
  4. 4
    过滤filtered
  5. 5
    浓缩concentrated under reduced pressure
  6. 6
    其他to provide a brown viscous liquid
  7. 7
    其他Purification

实验过程

In a round bottom flask, Compound 5 (2.2 g, 13×10−3 mol) is treated with a solution of K2CO3 (5.6 g, 40×10−3 mol, in 20 mL of water), with magnetic stirring at room temperature. The progress of the reaction is followed by TLC (eluent: ethyl acetate/methanol, 98/2). After stirring for 3.5 hrs, the reaction is complete. The reaction mixture is neutralized (pH=7) by adding 1N hydrochloric acid and then freeze-dried for 16 hrs. The organic residue is then extracted with CH2Cl2 (40 mL), filtered and then concentrated under reduced pressure to provide a brown viscous liquid. Purification was carried out on a silica gel column (eluent: ethyl acetate/methanol, 98/2). Compound 6 is obtained after such purification as a white powder.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08597706B2uspto-grants-2013_12