Methyl iodide → Hexanoic acid, 2-methoxy-

HRID 1393014

반응식

HRID 1393014 반응식
[OH:1][CH:2]([CH2:6][CH2:7][CH2:8][CH3:9])[C:3]([OH:5])=[O:4].[H-].[Na+].I[CH3:13]>C1COCC1>[CH3:13][O:1][CH:2]([CH2:6][CH2:7][CH2:8][CH3:9])[C:3]([OH:5])=[O:4]

참가 물질

5

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.

후처리

  1. stirringthe mixture was stirred at room temperature overnight
  2. customIt was quenched with water
  3. stirringstirred for 4 hours
  4. extractionThe mixture was extracted with 5% methanol in dichloromethane, organic layer
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-b94785ade18844cea214dd81f6112b64
출처 데이터셋
uspto-grants-2008_03
특허 번호
US07345034B2

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