4-(4-Fluoro-benzyloxy)-phthalic acid bis-(4-fluoro-benzyl) ester → 4-(4-Fluoro-benzyloxy)-phthalic acid

HRID 1070679노트

반응식

HRID 1070679 반응식
FC1C=CC(C[O:7][C:8](=[O:35])[C:9]2[C:10](=[CH:22][C:23]([O:26][CH2:27][C:28]3[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=3)=[CH:24][CH:25]=2)[C:11]([O:13]CC2C=CC(F)=CC=2)=[O:12])=CC=1>O1CCCC1.O>[F:34][C:31]1[CH:30]=[CH:29][C:28]([CH2:27][O:26][C:23]2[CH:22]=[C:10]([C:11]([OH:13])=[O:12])[C:9](=[CH:25][CH:24]=2)[C:8]([OH:35])=[O:7])=[CH:33][CH:32]=1

참가 물질

4

반응물 1

HCID 697368654-(4-Fluoro-benzyloxy)-phthalic acid bis-(4-fluoro-benzyl) ester

생성물 1

HCID 223970954-(4-Fluoro-benzyloxy)-phthalic acid수율 56%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 4-(4-fluoro-benzyloxy)-phthalic acid bis-(4-fluoro-benzyl) ester (7.8 g, 15.4 mmol) lithium hydroxide monohydrate (1.8 g, 46.2 mmol) in tetrahydrofuran (60 mL) and water (60 mL) was stirred at room temperature for 72 h. The mixture was then evaporated followed by acidification to pH 2 at 0° C. with concentrated HCl. The organic layer was then diluted with ethyl acetate, separared, washed with water and dried over sodium sulfate. Filtration and half evaporation gave a white suspension which was filtered off and washed with ether to afford the title compound (2.5 g, 56%) as a white solid.

후처리

  1. customThe mixture was then evaporated
  2. customfollowed by acidification to pH 2 at 0° C. with concentrated HCl
  3. additionThe organic layer was then diluted with ethyl acetate
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. filtrationFiltration and half evaporation
  7. customgave a white suspension which
  8. filtrationwas filtered off
  9. washwashed with ether

출처 및 근거

ORD 기록
ord-bd24580e823649e9b37825c97ec4df82
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06903095B2

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