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Dimethyl Sulfoxide → 2-Vinylanisole

HRID 1821658
ノート
印刷プレビュー

反応式

HRID 1821658 の反応式
[H-].[Na+].[CH3:3][O:4][C:5]1[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=1[CH:7]=O.[CH3:13]S(C)=O>[Br-].C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH3:3][O:4][C:5]1[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=1[CH:7]=[CH2:13]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 679Dimethyl Sulfoxide2 回HCID 86582-MethoxybenzaldehydeHCID 24758Sodium hydride

生成物 1

HCID 611532-Vinylanisole収率 61.1%

試薬・触媒・溶媒 1

HCID 74505Methyltriphenyliphosphonium bromide触媒

反応条件

温度
85 °C

実験手順

Under nitrogen atmosphere, in dry dimethylsulfoxide (15 mL) was suspended 1.92 g (48.0 mmol) of 60% sodium hydride washed with hexane, after stirring the suspension at 85° C. for 30 minutes, it was cooled to room temperature and then, in an ice bath, a dry dimethylsulfoxide (35 mL) solution containing 17.2 g (48.2 mmol) of methyl(triphenyl)phosphonium bromide was gradually added dropwise thereto. After stirring at room temperature for 20 minutes, 4.83 mL (40.1 mmol) of commercially available 2-methoxybenzaldehyde was added dropwise thereto, and the resulting mixture was stirred at room temperature for 1 hour and then at 65° C. for 3 hours. The reaction mixture was poured into ice water, and extracted with ethyl acetate. The organic layer was successively washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was removed, and the obtained residue was purified by silica gel column chromatography (Wako gel C-100, hexane-ethyl acetate, gradient) to obtain 3.29 g (24.5 mmol, Yield: 61.1%) of 1-methoxy-2-vinylbenzene.

後処理

  1. washwashed with hexane
  2. temperatureit was cooled to room temperature
  3. additionwas gradually added dropwise
  4. stirringAfter stirring at room temperature for 20 minutes
  5. stirringthe resulting mixture was stirred at room temperature for 1 hour
  6. waitat 65° C. for 3 hours
  7. extractionextracted with ethyl acetate
  8. washThe organic layer was successively washed with water and brine
  9. dry with materialdried over anhydrous magnesium sulfate
  10. customThe solvent was removed
  11. customthe obtained residue was purified by silica gel column chromatography (Wako gel C-100, hexane-ethyl acetate, gradient)

出典と根拠

ORDレコード
ord-dfabc9af3d104b81b5bb0166de1bc63e
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07608563B2

反応ノート

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