Lithium Hydroxide → HCID 18443662, 화합물

HRID 459148

반응식

HRID 459148 반응식
[OH-].[Li+].C[O:4][C:5](=[O:19])[CH:6]([O:17][CH3:18])[CH2:7][C:8]1[CH:13]=[CH:12][C:11]([OH:14])=[C:10]([O:15][CH3:16])[CH:9]=1>C1COCC1>[OH:14][C:11]1[CH:12]=[CH:13][C:8]([CH2:7][CH:6]([O:17][CH3:18])[C:5]([OH:19])=[O:4])=[CH:9][C:10]=1[O:15][CH3:16]

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 588230083-(4-Hydroxy-3-methoxy-phenyl)-2-methoxy-propionic acid methyl ester

생성물 1

HCID 18443662HCID 18443662, 화합물수율 74%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A 1N aqueous lithium hydroxide solution was added to a solution of 3-(4-hydroxy-3-methoxy-phenyl)-2-methoxy-propionic acid methyl ester (280 mg, 1.17 mmol) in THF at room temperature, and the reaction mixture stirred overnight. The aqueous phase was extracted with ethyl acetate (20 mL), acidified to pH 2, and extracted with ethyl acetate (3×15 mL). The later organic layers were combined and washed with water (15 mL) and brine (10 mL), dried (MgSO4), filtered, and concentrated under vacuum to produce 3-(4-hydroxy-3-methoxy-phenyl)-2-methoxy-propionic acid as an oil (183 mg, 74%). 1H-NMR (250.13 MHz, CDCl3): δ 6.83 (1H, d, J=7.8), 6.74 (1H, s), 6.72 (1H, d, J=7.8), 3.99 (1H dd, J=7.8, 4.0), 3.85 (s, 3H), 3.40 (s, 3H), 3.09 (1H, dd, J=14.2, 4.0), 2.91 (1H dd, J=14.2, 7.8).

후처리

  1. extractionThe aqueous phase was extracted with ethyl acetate (20 mL)
  2. extractionextracted with ethyl acetate (3×15 mL)
  3. washwashed with water (15 mL) and brine (10 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-2d4d67a8859f406389ddf0bfde39991c
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07192982B2

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