12-Methoxydodecanoate → Methyl 12-Methoxydodecanoate

HRID 342720

反応式

HRID 342720 の反応式
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]

参加物

5

反応物 3

HCID 142012-MethoxydodecanoateHCID 6328Methyl iodideHCID 82620Tetramethylammonium Hydroxide Pentahydrate

生成物 1

HCID 19611779Methyl 12-Methoxydodecanoate収率 98.8%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-eff937e8d2c84f949f022036a20c9d32
出典データセット
uspto-grants-1999_01
特許番号
US05859052

関連ノート

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