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

HRID 516819

반응식

HRID 516819 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-ed32896d4477471a8d470190ed294692
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115072B2

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