Hydrochloric Acid → Methyl 2-(4-chloromethylphenoxy)propionate

HRID 482428ノート

反応式

HRID 482428 の反応式
O[CH2:2][C:3]1[CH:15]=[CH:14][C:6]([O:7][CH:8]([CH3:13])[C:9]([O:11][CH3:12])=[O:10])=[CH:5][CH:4]=1.[ClH:16]>>[Cl:16][CH2:2][C:3]1[CH:15]=[CH:14][C:6]([O:7][CH:8]([CH3:13])[C:9]([O:11][CH3:12])=[O:10])=[CH:5][CH:4]=1

参加物

3

反応物 2

HCID 313Hydrochloric AcidHCID 18759642Methyl 2-(4-hydroxymethylphenoxy)propionate

生成物 1

HCID 18981037Methyl 2-(4-chloromethylphenoxy)propionate収率 67.3%

実験手順

A mixture of 2.19 g (0.0104 mole) of methyl 2-(4-hydroxymethylphenoxy)propionate and 3.00 g (0.0823 mole) of 36% hydrochloric acid was stirred for fifteen minutes at room temperature. The reaction mixture was then poured into ice-water, and the resulting mixture was extracted with diethyl ether. The extracts were combined and washed in succession with water and a saturated aqueous solution of sodium bicarbonate. The extract was dried over anhydrous magnesium sulfate and filtered, and the solvent was evaporated from the filtrate under reduced pressure, leaving a colorless liquid. This liquid was placed on a column of silica gel and eluted with methylene chloride. After the product-containing fractions were combined and the solvent evaporated under reduced pressure, 1.6 g of methyl 2-(4-chloromethylphenoxy)propionate was isolated as a colorless liquid. The NMR and IR spectra were consistent with the proposed structure.

後処理

  1. extractionthe resulting mixture was extracted with diethyl ether
  2. washwashed in succession with water
  3. dry with materialThe extract was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customthe solvent was evaporated from the filtrate under reduced pressure
  6. customleaving a colorless liquid
  7. washeluted with methylene chloride
  8. customthe solvent evaporated under reduced pressure

出典と根拠

ORDレコード
ord-0ba215519d9a4b7693dfc8df7fc551b3
出典データセット
uspto-grants-1998_08
特許番号
US05798316

反応ノート

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