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Thionyl Chloride → HCID 18955940、化合物

HRID 893292
ノート
印刷プレビュー

反応式

HRID 893292 の反応式
[Br:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[CH:4](O)[C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][CH:6]=1.S(Cl)([Cl:19])=O>ClCCl>[Br:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[CH:4]([Cl:19])[C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][CH:6]=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 12319462HCID 12319462、化合物

生成物 1

HCID 18955940HCID 18955940、化合物収率 76%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The crude benzhydryl alcohol from above (31.8 g, 107 mmole) was dissolved in 150 ml of dichloromethane and 11.7 ml (1.5 equiv.) of thionyl chloride was added dropwise over ten minutes. The solution was stirred overnight at room temperature and the solvent was removed under vacuum. The crude product was redissolved in 100 ml of toluene and the solvent was again removed under vacuum in order to eliminate excess thionyl chloride, providing crude product as a dark oil. The material was purified by short path distillation (Kugelrohr apparatus, 150° C., 0.5 mm) to give 25.8 g (76%) of (2-bromophenyl)chloro(4-chlorophenyl)methane as a pale yellow oil.

後処理

  1. customthe solvent was removed under vacuum
  2. dissolutionThe crude product was redissolved in 100 ml of toluene
  3. customthe solvent was again removed under vacuum in order
  4. customproviding crude product as a dark oil
  5. distillationThe material was purified by short path distillation (Kugelrohr apparatus, 150° C., 0.5 mm)

出典と根拠

ORDレコード
ord-6311c3b5acec452a84f62998ec59cedb
出典データセット
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05124330

反応ノート

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