Cesium carbonate → 3-Ethynyl-1,1'-biphenyl

HRID 271109ノート

反応式

HRID 271109 の反応式
[C:1]1([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:6]=[CH:5][CH:4]=[C:3]([C:7]#[C:8][Si](C)(C)C)[CH:2]=1.C([O-])([O-])=O.[Cs+].[Cs+]>CCO.C(Cl)Cl>[C:7]([C:3]1[CH:2]=[C:1]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:6]=[CH:5][CH:4]=1)#[CH:8]

参加物

4

反応物 2

HCID 10796Cesium carbonateHCID 59834575[([1,1'-Biphenyl]-3-yl)ethynyl](trimethyl)silane

生成物 1

HCID 127880263-Ethynyl-1,1'-biphenyl収率 91%

試薬・触媒・溶媒 1

HCID 21584144Dichloromethane ethanol溶媒

実験手順

To a solution of (1,1′-biphenyl-3-ylethynyl)(trimethyl)silane (4.74 g, 18.96) in 1/1 EtOH/CH2Cl2 (60 mL) is added Cs2CO3 (6.78 g, 20.85 mmol) at room temperature. After stirring for 1 h, the insoluble material is filtered off and the filtrate is concentrated. The crude material is purified by chromatography (silica gel, 100% hexane) to give the title compound (3.07 g, 91%) as an oil. MS (+) EI: 178 M+.

後処理

  1. filtrationthe insoluble material is filtered off
  2. concentrationthe filtrate is concentrated
  3. customThe crude material is purified by chromatography (silica gel, 100% hexane)

出典と根拠

ORDレコード
ord-72224c16d3a64c1ca9e66da71a12be05
出典データセット
uspto-grants-2008_11
特許番号
US07452885B2

反応ノート

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