Methyl iodide → 5-Methoxyadamantan-2-one

HRID 266040

反応式

HRID 266040 の反応式
[CH2:1]1[CH2:5][O:4][CH2:3][CH2:2]1.O[C:7]12[CH2:16]C3CC([CH2:15][CH:9]([C:10]3=[O:17])[CH2:8]1)[CH2:14]2.CI.[H-].[Na+]>O>[CH3:3][O:4][C:5]12[CH2:1][CH:2]3[CH2:14][CH:7]([CH2:8][CH:9]([C:10]3=[O:17])[CH2:15]1)[CH2:16]2

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 64184Idramantone

生成物 1

HCID 5283525-Methoxyadamantan-2-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

THF 5 ml solution of 5-hydroxy-2-adamantanone 100 mg and methyl iodide 0.113 ml was cooled at 0° C., and sodium hydride (60%, oil suspension) 48.2 mg was added therein, and the temperature of the reaction mixture was gradually changed to room temperature, then stirred for 25 hours. The reaction mixture was cooled again, and water was added thereto, then THF was removed by concentration in vacuo. The thus obtained residue was extracted with chloroform and dried by adding anhydrous sodium sulfate. After separation of the drying agent, the filtrate was concentrated in vacuo. Residue was purified by means of silica gel column chromatography (Wako gel, C200, n-hexane: ethyl acetate=10:1) to obtain the product.

後処理

  1. customwas gradually changed to room temperature
  2. temperatureThe reaction mixture was cooled again
  3. customTHF was removed by concentration in vacuo
  4. extractionThe thus obtained residue was extracted with chloroform
  5. customdried
  6. additionby adding anhydrous sodium sulfate
  7. customAfter separation of the drying agent
  8. concentrationthe filtrate was concentrated in vacuo
  9. customResidue was purified by means of silica gel column chromatography (Wako gel, C200, n-hexane: ethyl acetate=10:1)
  10. customto obtain the product

出典と根拠

ORDレコード
ord-1f05df81ea684a0eac2c1f6724f77769
出典データセット
uspto-grants-1997_07
特許番号
US05650406

関連ノート

読み込み中…