Cesium carbonate → 1-(Difluoromethoxy)-4-ethynylbenzene

HRID 646230

反応式

HRID 646230 の反応式
[F:1][CH:2]([F:16])[O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]#[C:11][Si](C)(C)C)=[CH:6][CH:5]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CCOCC.CCCCCC.C(Cl)Cl>[F:1][CH:2]([F:16])[O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]#[CH:11])=[CH:6][CH:5]=1

参加物

5

反応物 2

HCID 10796Cesium carbonateHCID 68699091{[4-(Difluoromethoxy)phenyl]ethynyl}(trimethyl)silane

生成物 1

HCID 27784971-(Difluoromethoxy)-4-ethynylbenzene収率 97%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 21584099Diethylether hexane溶媒

実験手順

A solution of {[4-(difluoromethoxy)phenyl]ethynyl}(trimethyl)silane (10.0 g, 41.7 mmol) in MeOH/CH2Cl2 (1/1) was treated with cesium carbonate (16.3 g, 50 mmol) at room temperature, stirred for 1.5 h, diluted with CH2Cl2 and filtered through a pad of silica gel. The filtrate was concentrated to dryness to give the title compound (6.8 g, 97%) as an oil, identified by NMR and mass spectral analyses. MS (+) EI:168.

後処理

  1. filtrationfiltered through a pad of silica gel
  2. concentrationThe filtrate was concentrated to dryness

出典と根拠

ORDレコード
ord-d89efcc5184c4c30883d065eed3cf3bf
出典データセット
uspto-grants-2010_04
特許番号
US07705030B2

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