Potassium Carbonate → 1-[(4-Ethynylphenoxy)methyl]-3-fluorobenzene

HRID 2184353ノート

反応式

HRID 2184353 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:19]=[CH:20][CH:21]=1)[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]#[C:14][Si](C)(C)C)=[CH:9][CH:8]=1.C(=O)([O-])[O-].[K+].[K+]>CO>[F:1][C:2]1[CH:3]=[C:4]([CH:19]=[CH:20][CH:21]=1)[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]#[CH:14])=[CH:9][CH:8]=1

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 22476627({4-[(3-Fluorophenyl)methoxy]phenyl}ethynyl)(trimethyl)silane

生成物 1

HCID 224766251-[(4-Ethynylphenoxy)methyl]-3-fluorobenzene

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 2.06 g (6.9 mmol) of [4-(3-fluoro-benzyloxy)-phenylethynyl]-trimethyl-silane in 35 ml methanol is treated with 95 mg (0.69 mmol) of solid potassium carbonate. The mixture is stirred at RT for 3 h, concentrated and treated with saturated aqueous sodium hydrogencarbonate. The compound is extracted three times with dichloromethane, dried over magnesium sulfate and concentrated to yield 1.53 g (98%) of a slightly brown oil. MS (neg.ions): m/e=225.4 (M−H).

後処理

  1. concentrationconcentrated
  2. additiontreated with saturated aqueous sodium hydrogencarbonate
  3. extractionThe compound is extracted three times with dichloromethane
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated
  6. customto yield 1.53 g (98%) of a slightly brown oil

出典と根拠

ORDレコード
ord-bc4eb899c74b4bd2ab2f8e5febe080d8
出典データセット
uspto-grants-2005_05
特許番号
US06900354B2

反応ノート

読み込み中…