Water → 2-Chloromethylbenzofuran

HRID 654757

反応式

HRID 654757 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[CH:3]=[C:2]1[CH2:10]O.S(Cl)([Cl:14])=O.O>C(Cl)(Cl)Cl.ClCCl>[Cl:14][CH2:10][C:2]1[O:1][C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[CH:3]=1

参加物

6

反応物 3

HCID 962WaterHCID 24386Thionyl ChlorideHCID 27762631-Benzofuran-2-Ylmethanol

生成物 1

HCID 1843482-Chloromethylbenzofuran収率 80%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒

実験手順

A three-necked flask is charged with 33.2 g of 2-benzofuranylmethanol dissolved in 450 ml of anhydrous chloroform, 48.8 ml of thionyl chloride are then introduced dropwise and the temperature is raised gently to reflux and maintained for 3 hours 30 minutes. The reaction medium is then cooled and poured into 1 1 of water, and is thereafter diluted with 500 ml of dichloromethane. After settling has taken place, the organic phase is washed to neutrality and dried over anhydrous magnesium sulfate, the solvent is evaporated off and the residue is distilled under vacuum to obtain the expected compound.

後処理

  1. temperaturethe temperature is raised gently
  2. temperatureto reflux
  3. temperaturemaintained for 3 hours 30 minutes
  4. temperatureThe reaction medium is then cooled
  5. washthe organic phase is washed to neutrality
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent is evaporated off
  8. distillationthe residue is distilled under vacuum

出典と根拠

ORDレコード
ord-48ea5c07afb64da1b9107fd6cb17100b
出典データセット
uspto-grants-1992_07
特許番号
US05134147

関連ノート

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