Methyl iodide → HCID 67304597、化合物

HRID 1009010ノート

反応式

HRID 1009010 の反応式
[H-].[Na+].[CH3:3][C:4]1[CH:8]=[CH:7][O:6][C:5]=1[CH2:9][OH:10].I[CH3:12]>O1CCCC1>[CH3:12][O:10][CH2:9][C:5]1[O:6][CH:7]=[CH:8][C:4]=1[CH3:3]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 11194308(3-methyl-2-furyl)methanol

生成物 1

HCID 67304597HCID 67304597、化合物収率 113.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Under an inert atmosphere sodium hydride (0.25 g ˜60%, 6.2 mmol, 1.1 equiv.) was suspended in dry tetrahydrofuran. At 5° C. a solution of (3-methyl-furan-2-yl)-methanol (0.63 g, 5.6 mmol) in dry tetrahydrofuran was added dropwise. The mixture was stirred at room temp. for one hour, then iodomethane (0.9 g, 6.2 mmol, 1.1 equiv.) was added dropwise. The mixture was stirred overnight at room temp., quenched with diluted acid and extracted with diethyl ether. The combined, organic extracts were washed with brine, dried over magnesium sulfate dihydrate, filtered and concentrated under reduced pressure to give 0.8 g of the title compound as a light yellow oil. GC-MS (EI): M=126.

後処理

  1. stirringThe mixture was stirred overnight at room temp.
  2. customquenched
  3. additionwith diluted acid
  4. extractionextracted with diethyl ether
  5. washorganic extracts were washed with brine
  6. dry with materialdried over magnesium sulfate dihydrate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-f0962129fe2648a0a9cc6bb8f2222eca
出典データセット
uspto-grants-2011_07
特許番号
US07973051B2

反応ノート

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