Triethylamine → 5-(Chloromethyl)-2,3-dihydro-1-benzofuran

HRID 7423ノート

反応式

HRID 7423 の反応式
[O:1]1[CH2:5][CH2:4][C:3]2[CH:6]=[C:7]([CH2:10]O)[CH:8]=[CH:9][C:2]1=2.C(N(CC)CC)C.CS([Cl:23])(=O)=O>ClCCl>[O:1]1[CH2:5][CH2:4][C:3]2[CH:6]=[C:7]([CH2:10][Cl:23])[CH:8]=[CH:9][C:2]1=2

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 2776158(2,3-Dihydro-1-benzofuran-5-yl)methanol

生成物 1

HCID 117896145-(Chloromethyl)-2,3-dihydro-1-benzofuran収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of (2,3-dihydrobenzo[b]furan-5-yl)methanol (1.5 g, 10 mmol) in dichloromethane (10 mL) were added under ice-cooling triethylamine (1.67 mL, 12 mmol) and methanesulfonyl chloride (0.85 mL, 10 mmol) and the mixture was stirred at room temperature for 1 h. The solvent was evaporated under reduced pressure and the obtained residue was dissolved in ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give an almost pure title compound (1.6 g, 100%).

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe obtained residue was dissolved in ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-481ec1a85eb24912b47c7efbb63a5f15
出典データセット
uspto-grants-2006_08
特許番号
US07087597B1

反応ノート

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