12-Methoxydodecanoate → Methyl 12-Methoxydodecanoate

HRID 1449765

반응식

HRID 1449765 반응식
O.O.O.O.O.[OH-].C[N+](C)(C)C.[CH3:12][O:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][C:25]([OH:27])=[O:26].[CH3:28]I>C(#N)C>[CH3:12][O:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][C:25]([O:27][CH3:28])=[O:26]

참가 물질

5

반응물 3

HCID 142012-MethoxydodecanoateHCID 6328Methyl iodideHCID 82620Tetramethylammonium Hydroxide Pentahydrate

생성물 1

HCID 19611779Methyl 12-Methoxydodecanoate수율 98.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Tetramethylammonium hydroxide pentahydrate (1.7 g, 9.4 mmol) was added to a solution of the title product of Example 1 (2.0 g, 8.7 mmol) in 45 mL of anhydrous acetonitrile. After stirring for 4 hours at room temperature, methyl iodide (0.6 mL, 9.6 mmol) was added and the resulting milky solution stirred at room temperature. The solvent was removed by rotary evaporator and partioned between diethyl ether and water. The organic phase was washed with brine, dried over magnesium sulfate, filtered and concentrated to give the title compound (2.1 g) as a pale yellow liquid. The structure was supported by NMR, infrared spectroscopy, elemental analysis and mass spectroscopy.

후처리

  1. stirringthe resulting milky solution stirred at room temperature
  2. customThe solvent was removed by rotary evaporator
  3. washThe organic phase was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f4aa2fdb6de248279b0af866db072ea8
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05599947

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