Dimethylformamide → Methyl 4-(4-oxo-4-phenylbutoxy)benzoate ethylene acetal

HRID 1585650

反応式

HRID 1585650 の反応式
[C:1]1([C:7]2([CH2:12][CH2:13][CH2:14]Cl)OCC[O:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:16](=[O:19])([O-])[O-].[K+].[K+].[OH:22][C:23]1[CH:32]=[CH:31][C:26]([C:27]([O:29][CH3:30])=[O:28])=[CH:25][CH:24]=1.[CH3:33]N(C)C=O>O>[CH2:16]1[O:19][C:27]([O:28][CH3:33])([C:26]2[CH:25]=[CH:24][C:23]([O:22][CH2:14][CH2:13][CH2:12][C:7](=[O:8])[C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)=[CH:32][CH:31]=2)[O:29][CH2:30]1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 7456MethylparabenHCID 11430Potassium CarbonateHCID 128663382-(3-Chloropropyl)-2-phenyl-1,3-dioxolane

生成物 1

HCID 70111092Methyl 4-(4-oxo-4-phenylbutoxy)benzoate ethylene acetal

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Crude 2-phenyl-2-(3-chloropropyl)-1,3-dioxolane (21.0 g), potassium carbonate (14.0 g; 0.101 moles) and methyl 4-hydroxybenzoate (14.0 g, 0.092 moles) were heated in dimethylformamide (100 ml) for 21 hours. The mixture was diluted with water (250 ml) and extracted with dichloromethane (500 ml). The dichloromethane extract was washed with saturated sodium bicarbonate solution and then with water. The organic extract was concentrated in vacuo to give the product as a brown solid (27.3 g).

後処理

  1. extractionextracted with dichloromethane (500 ml)
  2. extractionThe dichloromethane extract
  3. washwas washed with saturated sodium bicarbonate solution
  4. extractionThe organic extract
  5. concentrationwas concentrated in vacuo

出典と根拠

ORDレコード
ord-7132aa972471458f9d7cf03adf3145e6
出典データセット
uspto-grants-1999_08
特許番号
US05939447

関連ノート

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