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Sulfuric Acid → N-[2-Methyl-1-(naphthalen-2-yl)propan-2-yl]acetamide

HRID 1349440
ノート
印刷プレビュー

反応式

HRID 1349440 の反応式
[CH3:1][C:2](O)([CH3:14])[CH2:3][C:4]1[CH:13]=[CH:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=1.[C:16](#[N:18])[CH3:17].S(=O)(=O)(O)[OH:20].[OH-].[Na+]>C(O)(=O)C>[CH3:1][C:2]([NH:18][C:16](=[O:20])[CH3:17])([CH3:14])[CH2:3][C:4]1[CH:13]=[CH:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=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 6342AcetonitrileHCID 14798Sodium HydroxideHCID 107744191-(2-Naphthyl)-2-methyl-2-propanol

生成物 1

HCID 22382419N-[2-Methyl-1-(naphthalen-2-yl)propan-2-yl]acetamide

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To 2-methyl-1-(naphtahlen-2-yl)-2-propanol (500 mg) obtained in Step 7 were added acetonitrile (0.5 ml) and acetic acid (0.5 ml) in this order. After ice-cooling the mixture, sulfuric acid (0.5 ml) was added dropwise. The mixture was stirred under ice-cooling for 20 min and poured into a 1N aqueous sodium hydroxide solution, and the mixture was extracted with diethyl ether. The organic layer was washed with water, dried over sodium sulfate, and concentrated under reduced pressure. The obtained residue was subjected to recrystallization from ethyl acetate-n-hexane to give the title compound (303 mg).

後処理

  1. additionwas added dropwise
  2. temperaturecooling for 20 min
  3. extractionthe mixture was extracted with diethyl ether
  4. washThe organic layer was washed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe obtained residue was subjected to recrystallization from ethyl acetate-n-hexane

出典と根拠

ORDレコード
ord-a2c725a81d01455eb43c15df71c986da
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07211685B2

反応ノート

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