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Nitric Acid → N-[4-(2,2-dimethylpropyl)phenyl]acetamide

HRID 1424234
ノート
印刷プレビュー

反応式

HRID 1424234 の反応式
[CH2:1]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[C:2]([CH3:5])([CH3:4])[CH3:3].[N+:12]([O-])(O)=O.[C:16]([O:19]C(=O)C)(=O)[CH3:17]>CO.[Pd]>[CH2:1]([C:6]1[CH:7]=[CH:8][C:9]([NH:12][C:16](=[O:19])[CH3:17])=[CH:10][CH:11]=1)[C:2]([CH3:5])([CH3:4])[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

6

反応物 3

HCID 944Nitric AcidHCID 7918Acetic Anhydride3 回HCID 13877Benzene, (2,2-dimethylpropyl)-

生成物 1

HCID 825793N-[4-(2,2-dimethylpropyl)phenyl]acetamide収率 22%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

To a solution of neopentylbenzene (9.20 g, 62 mmol) in acetic anhydride (30 mL) cooled in an ice bath was slowly added a solution of nitric acid (3.5 mL, 83 mmol) in acetic anhydride (10 mL). The reaction was allowed to warm to room temperature for 18 hours. The yellow reaction mixture was added to ice water and extracted with diethylether (3×). The organic layers were combined, washed with brine, dried over anhydrous magnesium sulphate, filtered, and concentrated in vacuo. This provided a 1:1 mixture of ortho and para nitro substituted compounds as a yellow solid. To this yellow solid dissolved in methanol (100 mL) was added acetic anhydride (8.4 mL, 89 mmol) and 10% palladium on carbon (700 mg, 7 mmol) and the reaction mixture hydrogenated at a pressure of 40 psi for 3 hours. The reaction was filtered through celite, concentrated in vacuo, and purified by silica gel column chromatography eluting with a 0-50% ethyl acetate/hexanes gradient. This provided the title compound (2.79 g, 22%) as a white solid.

後処理

  1. extractionextracted with diethylether (3×)
  2. washwashed with brine
  3. dry with materialdried over anhydrous magnesium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThis provided
  7. additiona 1:1 mixture of ortho and para nitro substituted compounds as a yellow solid
  8. filtrationThe reaction was filtered through celite
  9. concentrationconcentrated in vacuo
  10. custompurified by silica gel column chromatography
  11. washeluting with a 0-50% ethyl acetate/hexanes gradient

出典と根拠

ORDレコード
ord-a5956302f971424e9e7e31976332d748
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08927587B2

反応ノート

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