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Nitric Acid → HCID 66745352、化合物

HRID 1175761
ノート
印刷プレビュー

反応式

HRID 1175761 の反応式
[O:1]=[C:2]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[O:8][C:4]2([CH2:7][CH2:6][CH2:5]2)[CH2:3]1.OS(O)(=O)=O.[N+:20]([O-])([OH:22])=[O:21]>C(O)(=O)C>[N+:20]([C:12]1[CH:13]=[CH:14][C:9]2[O:8][C:4]3([CH2:7][CH2:6][CH2:5]3)[CH2:3][C:2](=[O:1])[C:10]=2[CH:11]=1)([O-:22])=[O:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 944Nitric AcidHCID 1118Sulfuric Acid2 回HCID 58237899spiro[chroman-2,1'-cyclobutan]-4-one

生成物 1

HCID 66745352HCID 66745352、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of 3,4-Dihydro-4-oxo-spiro[2H-1-benzopyran-2,1′-cyclobutane] (Example 3) (10 mmol) in glacial acetic acid (2 ml), conc. H2SO4 (10 mmol) was added at 0° C. and the mixture was stirred for 10 min. A chilled nitrating mixture [prepared from HNO3 (9 mmol) and Conc. H2SO4 (10 mmol)] was then added very slowly and the reaction mixture was allowed to warm up to room temperature and stirred for 5 h. reaction mixture was then quenched with water and the compound was extracted in dichloromethane. Organic layer was separated, dried on anhydrous MgSO4 and concentrated under vacuum. The crude product was then purified by column chromatography to afford the desired compound as a yellow solid.

後処理

  1. additionwas then added very slowly
  2. stirringstirred for 5 h.
  3. customreaction mixture
  4. customwas then quenched with water
  5. extractionthe compound was extracted in dichloromethane
  6. customOrganic layer was separated
  7. dry with materialdried on anhydrous MgSO4
  8. concentrationconcentrated under vacuum
  9. customThe crude product was then purified by column chromatography

出典と根拠

ORDレコード
ord-8cdd20c896ac430e849544ca62a77598
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07842703B2

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