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Sodium borohydride → Ethyl {4-[9-(ethyloxy)-4-hydroxy-1-oxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl]-3-fluorophenyl}acetate

HRID 222436
ノート
印刷プレビュー

反応式

HRID 222436 の反応式
[CH2:1]([O:3][C:4]1[C:12]2[C:11](=[O:13])[N:10]([C:14]3[CH:19]=[CH:18][C:17]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:16][C:15]=3[F:26])[C:9](=O)[C:8]=2[C:7]([OH:28])=[C:6]2[CH:29]=[CH:30][CH:31]=[CH:32][C:5]=12)[CH3:2].[BH4-].[Na+]>C1COCC1>[CH2:1]([O:3][C:4]1[C:12]2[C:11](=[O:13])[N:10]([C:14]3[CH:19]=[CH:18][C:17]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:16][C:15]=3[F:26])[CH2:9][C:8]=2[C:7]([OH:28])=[C:6]2[CH:29]=[CH:30][CH:31]=[CH:32][C:5]=12)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 4311764Sodium borohydride3 回HCID 58012505Ethyl {4-[4-(ethyloxy)-9-hydroxy-1,3-dioxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl]-3-fluorophenyl}acetate

生成物 1

HCID 58231483Ethyl {4-[9-(ethyloxy)-4-hydroxy-1-oxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl]-3-fluorophenyl}acetate収率 101.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of ethyl {4-[4-(ethyloxy)-9-hydroxy-1,3-dioxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl]-3-fluorophenyl}acetate (2.50 g, 5.72 mmol) in THF (50 ml) under an argon atmosphere, was added sodium borohydride (0.217 g, 5.72 mmol) followed by borane THF complex solution (1.0M in THF, 5.72 ml, 5.72 mmol). This was stirred at room temperature for 2 hours. A further 5.72 mmol of sodium borohydride and borane THF complex was added to the reaction mixture and stirring continued for 2 hours. Finally, a further 2.86 mmol addition of sodium borohydride and borane THF complex was made and stirring continued for 1.5 hours until the reaction was complete. This was quenched with ethyl acetate (100 ml) and methanol (3 ml) then washed with 2N HCl (100 ml). The aqueous was re-extracted with ethyl acetate (200 ml). The combined organics were washed with brine (200 ml), dried over magnesium sulphate, filtered and evaporated to give the title compound as a pale yellow solid (2.45 g, 5.79 mmol).

後処理

  1. stirringstirring
  2. waitcontinued for 2 hours
  3. stirringstirring
  4. waitcontinued for 1.5 hours until the reaction
  5. customThis was quenched with ethyl acetate (100 ml) and methanol (3 ml)
  6. washthen washed with 2N HCl (100 ml)
  7. extractionThe aqueous was re-extracted with ethyl acetate (200 ml)
  8. washThe combined organics were washed with brine (200 ml)
  9. dry with materialdried over magnesium sulphate
  10. filtrationfiltered
  11. customevaporated

出典と根拠

ORDレコード
ord-c92bf9c790674d8db3865294738c3db8
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08207213B2

反応ノート

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