Methylparaben → HCID 54331531、化合物

HRID 1788770ノート

反応式

HRID 1788770 の反応式
[CH3:1][O:2][C:3](=[O:11])[C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1.[CH2:12]([CH:14]([CH2:17][CH2:18][CH2:19][CH3:20])[CH2:15]Cl)[CH3:13].C[O-].[Na+]>CN(C)C=O>[CH3:1][O:2][C:3](=[O:11])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:15][CH:14]([CH2:12][CH3:13])[CH2:17][CH2:18][CH2:19][CH3:20])=[CH:6][CH:5]=1

参加物

5

反応物 3

HCID 7456MethylparabenHCID 312402-Ethylhexyl chlorideHCID 10942334Sodium Methoxide

生成物 1

HCID 54331531HCID 54331531、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 51.7 g (0.34 mol) of 4-hydroxybenzoic acid methylester, 500 ml of dimethyl formamide, 60 g (0.40 mol) of 2-ethylhexylchloride and 21.8 g (0.40 mol) of sodium methylate was heated for 7 hours to boiling temperature and, after cooling and removal of the sodium chloride by filtration, was evaporated to dryness under reduced pressure. The residue was dissolved in methylene chloride and chromatographed (eluent: methylene chloride) on silica gel (Merck) to yield 43 g (48% of the theoretical) of 4-(2-ethylhexyloxy)benzoic acid methylester. A refractive index of

後処理

  1. temperaturewas heated for 7 hours
  2. temperatureafter cooling
  3. customremoval of the sodium chloride
  4. filtrationby filtration
  5. customwas evaporated to dryness under reduced pressure
  6. dissolutionThe residue was dissolved in methylene chloride
  7. customchromatographed (eluent: methylene chloride) on silica gel (Merck)

出典と根拠

ORDレコード
ord-145a27aebfd74767a69e19e03a8c59f6
出典データセット
uspto-grants-1987_08
特許番号
US04684665

反応ノート

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