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

HRID 1070679ノート

反応式

HRID 1070679 の反応式
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

参加物

4

反応物 1

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

生成物 1

HCID 223970954-(4-Fluoro-benzyloxy)-phthalic acid収率 56%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bd24580e823649e9b37825c97ec4df82
出典データセット
uspto-grants-2005_06
特許番号
US06903095B2

反応ノート

読み込み中…