Phosphorus tribromide → 3-(6-Bromo-3-bromomethyl-2-fluoro-phenoxy)-5-chloro-benzonitrile

HRID 559057ノート

反応式

HRID 559057 の反応式
P(Br)(Br)[Br:2].[Br:5][C:6]1[C:11]([O:12][C:13]2[CH:14]=[C:15]([CH:18]=[C:19]([Cl:21])[CH:20]=2)[C:16]#[N:17])=[C:10]([F:22])[C:9]([CH2:23]O)=[CH:8][CH:7]=1>C(Cl)Cl>[Br:5][C:6]1[C:11]([O:12][C:13]2[CH:14]=[C:15]([CH:18]=[C:19]([Cl:21])[CH:20]=2)[C:16]#[N:17])=[C:10]([F:22])[C:9]([CH2:23][Br:2])=[CH:8][CH:7]=1

参加物

4

反応物 2

HCID 24614Phosphorus tribromideHCID 669992083-(6-Bromo-2-fluoro-3-hydroxymethyl-phenoxy)-5-chloro-benzonitrile

生成物 1

HCID 669997373-(6-Bromo-3-bromomethyl-2-fluoro-phenoxy)-5-chloro-benzonitrile収率 60%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of PBr3 (0.74 mL of a 1 M solution in DCM, 1.1 equiv) was added to a solution of 107 (0.24 g, 0.67 mmol) in DCM (5 mL). The mixture was stirred at RT for 1 h and then concentrated in vacuo. The residue was dissolved in EtOAc, washed with saturated aqueous NaHCO3, and dried (MgSO4). Evaporation of the volatile materials afforded 0.17 g (60%) of 96.

後処理

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residue was dissolved in EtOAc
  3. washwashed with saturated aqueous NaHCO3
  4. dry with materialdried (MgSO4)
  5. customEvaporation of the volatile materials

出典と根拠

ORDレコード
ord-bcc8d59da0a64c44993373471a9d8321
出典データセット
uspto-grants-2011_11
特許番号
US08063064B2

反応ノート

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