3-Hydroxy-4-methoxybenzeneacetic acid → Ethyl 2-(3-hydroxy-4-methoxyphenyl)acetate

HRID 516819

反応式

HRID 516819 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH2:10][C:11]([OH:13])=[O:12])[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].O.[C:15]1(C)C=CC(S(O)(=O)=O)=C[CH:16]=1>C(O)C>[OH:1][C:2]1[CH:3]=[C:4]([CH2:10][C:11]([O:13][CH2:15][CH3:16])=[O:12])[CH:5]=[CH:6][C:7]=1[O:8][CH3:9]

参加物

4

反応物 2

HCID 1605623-Hydroxy-4-methoxybenzeneacetic acidHCID 521998p-Toluenesulfonic acid monohydrate

生成物 1

HCID 5324706Ethyl 2-(3-hydroxy-4-methoxyphenyl)acetate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The stirred solution of 2-(3-Hydroxy-4-methoxyphenyl)acetic acid (9.82 g, 53.90 mmol) and p-Toluenesulfonic acid monohydrate (1.15 g, 6.0 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. 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
  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-ed32896d4477471a8d470190ed294692
出典データセット
uspto-grants-2015_08
特許番号
US09115072B2

関連ノート

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