(2-Hydroxyphenyl)acetic acid → 2-(2-Hydroxyphenyl)acetic acid ethyl ester

HRID 73466

反応式

HRID 73466 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][C:9]([OH:11])=[O:10].O.[C:13]1(C)C=CC(S(O)(=O)=O)=C[CH:14]=1>C(O)C>[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][C:9]([O:11][CH2:13][CH3:14])=[O:10]

参加物

4

反応物 2

HCID 11970(2-Hydroxyphenyl)acetic acidHCID 521998p-Toluenesulfonic acid monohydrate

生成物 1

HCID 5210752-(2-Hydroxyphenyl)acetic acid ethyl ester

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The stirred solution of 2-(2-Hydroxyphenyl)acetic acid (10 g, 65.7 mmol) and p-Toluenesulfonic acid monohydrate (1.40 g, 7.3 mmol) in abs ethanol (100 ml) was refluxed for 4 hours or until all the starting material is consumed. The reaction mixture was concentrated, diluted with ethyl acetate and washed with 1M HCl and brine. The organic layer was dried over Na2SO4, filtered, concentrated, and purified by flash chromatography on a silica gel column (hex:ethyl acetate 2:1) to give the title compound.

後処理

  1. customis consumed
  2. concentrationThe reaction mixture was concentrated
  3. additiondiluted with ethyl acetate
  4. washwashed with 1M HCl and brine
  5. dry with materialThe organic layer was dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. custompurified by flash chromatography on a silica gel column (hex:ethyl acetate 2:1)

出典と根拠

ORDレコード
ord-3444b0344ac24d3e987a63805847d5ac
出典データセット
uspto-grants-2014_09
特許番号
US08829058B2

関連ノート

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