반응 #1331379

ord-1c6d879ab46c45bfb06fb50f1cb25cab

반응 방정식

O=C1CCC(=O)N1
succinimide
CCO
ethanol
O=B[O-].[Na+]
sodium boranate
[K+].[OH-]
potassium hydroxide
CCOC1CCC(=O)N1
γ-ethoxy-γ-butyrolactam
수율 55.0%

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGthe mixture was stirred for a further 15 minutes
  2. 2
    기타evaporated
  3. 3
    추출extracted three times with dichloromethane
  4. 4
    건조After drying over sodium sulphate
  5. 5
    농축concentrating

실험 절차

At 0° C., 9.91 g of succinimide were charged initially in 415 ml of ethanol and a total of 5.53 g of sodium boranate was added a little at a time. At this temperature, every 15 minutes 2 to 3 drops of 2N ethanolic hydrogen chloride were added dropwise over 4½ hours. Subsequently, the mixture was acidified to pH 3 using more acid. After stirring for 1 hour at 0° C., the mixture was neutralized using 1% strength ethanolic potassium hydroxide solution and the mixture was stirred for a further 15 minutes and evaporated. The residue was taken up in water and extracted three times with dichloromethane. After drying over sodium sulphate and concentrating, 7.16 g (55% of theory) of γ-ethoxy-γ-butyrolactam were obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07122506B2uspto-grants-2006_10