Sulfuric Acid → 1-Diethylamino-6-(m-methoxyphenyl)heptan-3-one

HRID 1414949ノート

反応式

HRID 1414949 の反応式
[CH2:1]([N:3]([CH2:19][CH3:20])[CH2:4][C:5]#[C:6][CH2:7][CH2:8][CH:9]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([O:17][CH3:18])[CH:12]=1)[CH3:10])[CH3:2].S(=O)(=O)(O)[OH:22]>>[CH2:19]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][C:6](=[O:22])[CH2:7][CH2:8][CH:9]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([O:17][CH3:18])[CH:12]=1)[CH3:10])[CH3:20]

参加物

3

反応物 2

HCID 1118Sulfuric AcidHCID 214856761-Diethylamino-6-(m-methoxyphenyl)hept-2-yne

生成物 1

HCID 214857581-Diethylamino-6-(m-methoxyphenyl)heptan-3-one

実験手順

Dissolve 1-diethylamino-6-(m-methoxyphenyl)hept-2-yne (13.6 g) in 10% aqueous sulphuric acid (40 cc) and stir with mercuric sulphate (0.69 g) for 2 hours at 70°. Filter the cooled solution, make basic with 10% aqueous sodium hydroxide and extract with ether. Wash the ethereal solution with water and brine, and dry (Na2SO4). Evaporate the solvent and distil the residue to obtain 1-diethylamino-6-(m-methoxyphenyl)heptan-3-one which has partially eliminated to 6-(m-methoxyphenyl)hept-1-en-3-one during the distillation, b.p. 145°/12 mm Hg.

後処理

  1. filtrationFilter the cooled solution
  2. extractionextract with ether
  3. washWash the ethereal solution with water and brine
  4. dry with materialdry (Na2SO4)
  5. customEvaporate the solvent
  6. customdistil the residue

出典と根拠

ORDレコード
ord-58e097e77bc84ba4bfe6bb2e51ca2961
出典データセット
uspto-grants-1977_01
特許番号
US04002746

反応ノート

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