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Thionyl Chloride → (E)-3-[4-(pyridin-3-ylmethyl)phenyl]allyl chloride hydrochloride

HRID 569146
ノート
印刷プレビュー

反応式

HRID 569146 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][C:8]2[CH:13]=[CH:12][C:11](/[CH:14]=[CH:15]/[CH2:16]O)=[CH:10][CH:9]=2)[CH:2]=1.S(Cl)([Cl:20])=O>C(Cl)Cl>[ClH:20].[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][C:8]2[CH:13]=[CH:12][C:11](/[CH:14]=[CH:15]/[CH2:16][Cl:20])=[CH:10][CH:9]=2)[CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 15594566(E)-3-[4-(pyridin-3-ylmethyl)phenyl]allyl alcohol

生成物 1

HCID 14099894(E)-3-[4-(pyridin-3-ylmethyl)phenyl]allyl chloride hydrochloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In 100 ml of methylene chloride was dissolved 10.5 g of (E)-3-[4-(pyridin-3-ylmethyl)phenyl]allyl alcohol, and 17 ml of thionyl chloride was added dropwise to the resulting solution with ice-cooling, after which the resulting mixture was subjected to reaction under reflux for 30 minutes. The solvent and the excessive thionyl chloride were removed by distillation under reduced pressure, to obtain (E)-3-[4-(pyridin-3-ylmethyl)phenyl]allyl chloride hydrochloride as the residue. This residue was dissolved in 40 ml of dimethyl sulfoxide.

後処理

  1. additionwas added dropwise to the resulting solution with ice-
  2. temperaturecooling
  3. customafter which the resulting mixture was subjected to reaction
  4. temperatureunder reflux for 30 minutes
  5. customThe solvent and the excessive thionyl chloride were removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-c1c60f60c303418e984f1ffc34df4d5a
出典データセット
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04731370

反応ノート

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