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Methylparaben → Methyl 4-(2-chloroethoxy)benzoate

HRID 354066
ノート
印刷プレビュー

反応式

HRID 354066 の反応式
[Na].[CH3:2][O:3][C:4](=[O:12])[C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][CH:6]=1.Br[CH2:14][CH2:15][Cl:16]>C(O)C>[CH3:2][O:3][C:4](=[O:12])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:14][CH2:15][Cl:16])=[CH:7][CH:6]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7456MethylparabenHCID 78491-Bromo-2-ChloroethaneHCID 5360545Sodium2 回

生成物 1

HCID 6485431Methyl 4-(2-chloroethoxy)benzoate収率 56.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
60 °C

実験手順

To 35 mL of ethanol was added sodium pellets (2.27gm, 98.6 mmol). After all the sodium had disappeared methyl-4-hydroxybenzoate (15 gm, 98 mmol) was added in one portion at room temperature. The reaction mixture was then heated to 60° C. and treated dropwise with 1-bromo-2-chloroethane (10.2 gm, 123 mmol) in 15 mL of ethanol. The reaction was stirred for 16 hrs then cooled to room temperature and concentrated. The residue was taken up in ethyl acetate and washed with water, 2N NaOH, and brine. The organic layer was dried over anhydrous magnesium sulfate, filtered, and concentrated. The crude product was chromatographed on silica gel using 1:10 Ethyl acetate:Hexanes to 1:6 Ethyl acetate:Hexanes as the gradient eluant to yield 11.9 gm of the title compound.

後処理

  1. additionwas added in one portion at room temperature
  2. temperaturethen cooled to room temperature
  3. concentrationconcentrated
  4. washwashed with water, 2N NaOH, and brine
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe crude product was chromatographed on silica gel using 1:10 Ethyl acetate

出典と根拠

ORDレコード
ord-7d754fc805774c178119e526a8db3322
出典データセット
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06756388B1

反応ノート

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