Nitric Acid → 4-Methyl-1-nitronaphthalene

HRID 1166787

反応式

HRID 1166787 の反応式
[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][CH:3]=1.OS(O)(=O)=O.[N+:17]([O-])([OH:19])=[O:18]>C(OCC)(=O)C>[N+:17]([C:5]1[C:6]2[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:2]([CH3:1])=[CH:3][CH:4]=1)([O-:19])=[O:18]

参加物

5

反応物 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 70021-Methylnaphthalene

生成物 1

HCID 701554-Methyl-1-nitronaphthalene

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a cold (0° C.) suspension of 1-methylnaphthalene (5 g) in HNO3 was added H2SO4 (5 mL) dropwise. After stirring the reaction for one hour, the solution was diluted with ethyl acetate and washed with water (3×), aqueous saturated NaHCO3 (2×) and brine, dried over MgSO4, and concentrated. The product was purified by silica gel column chromatography using ethyl acetate:hexane (5:95) and recrystallized from methanol to give yellow needles.

後処理

  1. customthe reaction for one hour
  2. washwashed with water (3×), aqueous saturated NaHCO3 (2×) and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe product was purified by silica gel column chromatography
  6. customrecrystallized from methanol
  7. customto give yellow needles

出典と根拠

ORDレコード
ord-c0acf37e673345a29bf4550df46cc2ac
出典データセット
uspto-grants-2003_09
特許番号
US06613942B1

関連ノート

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