Lithium Hydroxide → 3-(Methoxyimino)-3-(4-methoxyphenyl)propanoic acid

HRID 133789노트

반응식

HRID 133789 반응식
[CH3:1][O:2][N:3]=[C:4]([C:11]1[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=1)[CH2:5][C:6]([O:8]CC)=[O:7].[OH-].[Li+]>C1COCC1>[CH3:1][O:2][N:3]=[C:4]([C:11]1[CH:12]=[CH:13][C:14]([O:17][CH3:18])=[CH:15][CH:16]=1)[CH2:5][C:6]([OH:8])=[O:7]

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 58984518Ethyl 3-(methoxyimino)-3-(4-methoxyphenyl)propanoate

생성물 1

HCID 589845323-(Methoxyimino)-3-(4-methoxyphenyl)propanoic acid

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of ethyl 3-(methoxyimino)-3-(4-methoxyphenyl)propanoate from Step A in THF (5 mL) was added 1 N lithium hydroxide (5 mL), and the resulting solution was stirred at room temperature for 12 h. Most of the solvents were removed in vacuo, and 1N hydrochloric acid (5 mL) was added. The aqueous layer was extrated with ethyl acetate (x4), and the combined organic layers were washed with brine, dried over anhydrous sodium sulfate, and filtered. The filtrate was evaporated in vacuo to give the title compound as a white solid (350 mg). 1H NMR (400 MHz, CDCl3) δ 7.58 (m), 6.89 (m), 4.00 (s), 3.96 (3), 3.81 (s), and 3.78 (s).

후처리

  1. customMost of the solvents were removed in vacuo, and 1N hydrochloric acid (5 mL)
  2. additionwas added
  3. washthe combined organic layers were washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. customThe filtrate was evaporated in vacuo

출처 및 근거

ORD 기록
ord-7040cc2b665f4e909153f74ea3074a02
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07390925B2

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