4-Methoxyphenol → Ethyl 2,2-bis(4-methoxyphenoxy)-acetate

HRID 28113

反応式

HRID 28113 の反応式
[Na].[CH3:2][O:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1.Cl[CH:12](Cl)[C:13]([O:15][CH2:16][CH3:17])=[O:14]>C(O)C.C(OCC)C>[CH3:2][O:3][C:4]1[CH:9]=[CH:8][C:7]([O:10][CH:12]([O:10][C:7]2[CH:8]=[CH:9][C:4]([O:3][CH3:2])=[CH:5][CH:6]=2)[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:6][CH:5]=1

参加物

6

反応物 3

HCID 90154-MethoxyphenolHCID 10808Ethyl dichloroacetateHCID 5360545Sodium

生成物 1

HCID 23338925Ethyl 2,2-bis(4-methoxyphenoxy)-acetate収率 76.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒4 回HCID 3283Diethyl Ether溶媒

実験手順

Sodium (5.4 g) is dissolved in absolute ethanol (160 cc). 4-Methoxyphenol (29.2 g) dissolved in absolute ethanol (20 cc) is added. The mixture is stirred for 1 hour at ambient temperature. Ethyl 2,2-dichloro-acetate (20 g) dissolved in absolute ethanol (20 cc) is then added and the mixture is heated under reflux for 20 hours. The ethanol is driven off under reduced pressure (20 mmHg) at 40° C. and the residue is taken up in diethyl ether (100 cc). The organic phase is washed with 0.1 N sodium hydroxide solution (100 cc) and with water (2×100 cc) and is then dried over sodium sulphate, filtered and concentrated to dryness under reduced pressure (20 mmHg) at 40° C. Ethyl 2,2-bis(4-methoxyphenoxy)-acetate (30 g) is thus obtained in the form of an oil.

後処理

  1. additionis added
  2. additionis then added
  3. temperaturethe mixture is heated
  4. temperatureunder reflux for 20 hours
  5. customis driven off under reduced pressure (20 mmHg) at 40° C.
  6. washThe organic phase is washed with 0.1 N sodium hydroxide solution (100 cc) and with water (2×100 cc)
  7. dry with materialis then dried over sodium sulphate
  8. filtrationfiltered
  9. concentrationconcentrated to dryness under reduced pressure (20 mmHg) at 40° C

出典と根拠

ORDレコード
ord-35ec60e01e794f74b58a8468a258b6f8
出典データセット
uspto-grants-1980_09
特許番号
US04225589

関連ノート

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