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Potassium Carbonate → 4-Tert-butyl-1-ethynyl-2-nitrobenzene

HRID 68451
ノート
印刷プレビュー

反応式

HRID 68451 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11]#[C:12][Si](C)(C)C)=[C:7]([N+:17]([O-:19])=[O:18])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+]>CO>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11]#[CH:12])=[C:7]([N+:17]([O-:19])=[O:18])[CH:6]=1)([CH3:4])([CH3:2])[CH3:3]
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 58016188(4-tert-Butyl-2-nitro-phenylethynyl)-trimethyl-silane

生成物 1

HCID 580162084-Tert-butyl-1-ethynyl-2-nitrobenzene収率 81.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

(4-tert-Butyl-2-nitro-phenylethynyl)-trimethyl-silane (3.167 g, 11.51 mmol) and potassium carbonate (3.18 g, 23.0 mmol) were stirred in 75 mL methanol for 20 minutes. The resulting mixture was partitioned between ethylacetate and water. The ethylacetate layer was washed with brine, dried over anhydrous MgSO4, concentrated in vacuo, and purified by flash chromatography with gradient elution with 0 to 5% ethylacetate/hexanes to yield 4-tert-Butyl-1-ethynyl-2-nitro-benzene (1.910 g, 9.398 mmol).

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

後処理

  1. customThe resulting mixture was partitioned between ethylacetate and water
  2. washThe ethylacetate layer was washed with brine
  3. dry with materialdried over anhydrous MgSO4
  4. concentrationconcentrated in vacuo
  5. custompurified by flash chromatography with gradient elution with 0 to 5% ethylacetate/hexanes

出典と根拠

ORDレコード
ord-8b5bd90862674a7f81336624c6c2e720
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822457B2

反応ノート

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