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Sulfuric Acid → tert-Butyl 3-oxocyclohexanecarboxylate

HRID 521176
ノート
印刷プレビュー

反応式

HRID 521176 の反応式
[O-]S([O-])(=O)=O.[Mg+2].S(=O)(=O)(O)O.[O:12]=[C:13]1[CH2:18][CH2:17][CH2:16][CH:15]([C:19]([OH:21])=[O:20])[CH2:14]1.[CH3:22][C:23](O)([CH3:25])[CH3:24]>C(Cl)Cl>[O:12]=[C:13]1[CH2:18][CH2:17][CH2:16][CH:15]([C:19]([O:21][C:23]([CH3:25])([CH3:24])[CH3:22])=[O:20])[CH2:14]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 6386tert-ButanolHCID 24083Sulfuric acid magnesium salt (1:1)HCID 27602523-Oxocyclohexane-1-carboxylic acid

生成物 1

HCID 66791571tert-Butyl 3-oxocyclohexanecarboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Anhydrous MgSO4 (3.4 g, 28 mmol) was suspended in DCM (28.1 mL) and to this vigorously stirred mixture was added concentrated sulfuric acid (0.7 g, 7 mmol). The resulting mixture was allowed to stir at ambient temperature for 30 minutes. 3-Oxocyclohexanecarboxylic acid (1.0 g, 7.0 mmol) was added followed by t-BuOH (2.6 g, 35 mmol). The resulting mixture was allowed to stir for 24 hours before it was filtered and flushed with DCM. The filtrate was washed with water, and the organic layer was again washed with water, brine, dried over anhydrous MgSO4, filtered, and concentrated in vacuo to afford the title compound. The residue was used without further purification.

後処理

  1. stirringto stir for 24 hours before it
  2. filtrationwas filtered
  3. customflushed with DCM
  4. washThe filtrate was washed with water
  5. washthe organic layer was again washed with water, brine
  6. dry with materialdried over anhydrous MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-cb3547b2d63a460d8f03752576650623
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09328099B2

反応ノート

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