반응 #1480196

ord-b94785ade18844cea214dd81f6112b64

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGthe mixture was stirred at room temperature overnight
  2. 2
    기타It was quenched with water
  3. 3
    workup.STIRRINGstirred for 4 hours
  4. 4
    추출The mixture was extracted with 5% methanol in dichloromethane, organic layer
  5. 5
    건조dried over sodium sulfate
  6. 6
    여과filtered
  7. 7
    농축the filtrate was concentrated

실험 절차

2-Hydroxy caproic acid (152 mg, 1.15 mmol) was dissolved in 3 mL anhydrous THF. Sodium hydride (95%, 61 mg, 2.41 mmol) was added and the mixture was stirred at room temperature for 40 min. Iodomethane (0.7 mL) was added and the mixture was stirred at room temperature overnight. It was quenched with water, stirred for 4 hours to hydrolyze the methyl ester, and then adjusted to pH 4 with 10% citric acid. The mixture was extracted with 5% methanol in dichloromethane, organic layer dried over sodium sulfate, filtered, and the filtrate was concentrated to give the crude 2-methoxy caproic acid which was used in next step without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07345034B2uspto-grants-2008_03