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Triethylamine → m-Phenoxybenzyl cyanide

HRID 584352
ノート
印刷プレビュー

反応式

HRID 584352 の反応式
[O:1]([C:8]1[CH:9]=[C:10]([CH:13]=[CH:14][CH:15]=1)[CH2:11]O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:16]([N:18](CC)CC)C>C(OCC)(=O)C.CS(Cl)(=O)=O>[O:1]([C:8]1[CH:9]=[C:10]([CH2:11][C:16]#[N:18])[CH:13]=[CH:14][CH:15]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 8471TriethylamineHCID 262953-Phenoxybenzyl alcohol

生成物 1

HCID 40075m-Phenoxybenzyl cyanide収率 32%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 31297Methanesulfonyl chloride溶媒

実験手順

To a solution of 3-phenoxybenzylalcohol (25.0 g) and triethylamine (26.3 ml) in ethyl acetate (300 ml), methanesulfonyl chloride (14.6 ml) was added dropwise at 0° C. After stirring for 1 hour, the reaction mixture was washed with saturated aqueous sodium chloride, dried (MgSO4) and concentrated. The residue was dissolved in acetone (300 ml), admixed with sodium iodide (37.5 g) and then stirred for 1 hour. The reaction mixture was concentrated, and the residue was diluted with water and then extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4), and then concentrated. The residue was dissolved in dimethyl sulfoxide (100 ml) and stirred with sodium cyanide (7.35 g) for 15 hours at room temperature. The reaction mixture was diluted with ethyl acetate, washed with water, dried (MgSO4), and then concentrated. The residue was subjected to column chromatography on silica gel to obtain 3-phenoxyphenylacetonitrile (8.36 g, yield 32%) as an oil from a fraction eluted with ethyl acetate-hexane (1:7. v/v).

後処理

  1. washthe reaction mixture was washed with saturated aqueous sodium chloride
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated
  4. dissolutionThe residue was dissolved in acetone (300 ml)
  5. stirringstirred for 1 hour
  6. concentrationThe reaction mixture was concentrated
  7. additionthe residue was diluted with water
  8. extractionextracted with ethyl acetate
  9. washThe ethyl acetate layer was washed with water
  10. dry with materialdried (MgSO4)
  11. concentrationconcentrated
  12. dissolutionThe residue was dissolved in dimethyl sulfoxide (100 ml)
  13. stirringstirred with sodium cyanide (7.35 g) for 15 hours at room temperature
  14. additionThe reaction mixture was diluted with ethyl acetate
  15. washwashed with water
  16. dry with materialdried (MgSO4)
  17. concentrationconcentrated

出典と根拠

ORDレコード
ord-641bab9e2a0943d386ef1cd4bfeb9dbd
出典データセット
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06924300B2

反応ノート

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