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Potassium Carbonate → HCID 50998807、化合物

HRID 882083
ノート
印刷プレビュー

反応式

HRID 882083 の反応式
[CH3:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:12]#[C:13][Si](C)(C)C)[CH:8]=2)[N:3]=1.C([O-])([O-])=O.[K+].[K+]>CO>[C:12]([C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][CH:6]=1)[N:3]=[C:2]([CH3:1])[CH:11]=[CH:10]2)#[CH:13]
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 11430Potassium CarbonateHCID 673240081315248-52-2

生成物 1

HCID 50998807HCID 50998807、化合物収率 98.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 2-methyl-6-trimethylsilanylethynyl-quinoline (2.1 g, 1.03 mmol, 1 eq) in solution in MeOH (5 mL) was added K2CO3 (5.69 g, 4.12 mmol, 4 eq), and the resulting mixture was stirred overnight at room temperature. The solvent was then removed under reduced pressure and water was then added. The aqueous layer was extracted twice with cyclohexane, and then the combined organic layers were washed with brine and dried over MgSO4. After filtration and concentration under reduced pressure the crude product was purified by column chromatography on silica gel (Cyclohexane-EtOAc 99:1) to afford 169 mg of 6-ethynyl-2-methyl-quinoline as a yellow crystal (98%).

後処理

  1. customThe solvent was then removed under reduced pressure and water
  2. additionwas then added
  3. extractionThe aqueous layer was extracted twice with cyclohexane
  4. washthe combined organic layers were washed with brine
  5. dry with materialdried over MgSO4
  6. filtrationAfter filtration and concentration under reduced pressure the crude product
  7. customwas purified by column chromatography on silica gel (Cyclohexane-EtOAc 99:1)

出典と根拠

ORDレコード
ord-57aa7445e11941299bfd5de5c58b7fbc
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08993767B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート