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Benzoic acid, 3-methyl-, methyl ester → 2-(4-methylbenzyl)-3-m-tolyl-2H-isoquinolin-1-one

HRID 915368
ノート
印刷プレビュー

反応式

HRID 915368 の反応式
C(NC(C)C)(C)C.C([Li])CCC.C([N-]C(C)C)(C)C.[Li+].[CH3:21][C:22]1[CH:38]=[CH:37][CH:36]=[CH:35][C:23]=1[C:24]([NH:26][CH2:27][C:28]1[CH:33]=[CH:32][C:31]([CH3:34])=[CH:30][CH:29]=1)=[O:25].CO[C:41](=O)[C:42]1[CH:47]=[CH:46][CH:45]=[C:44]([CH3:48])[CH:43]=1>C1COCC1.CCCCCC>[CH3:34][C:31]1[CH:30]=[CH:29][C:28]([CH2:27][N:26]2[C:41]([C:42]3[CH:43]=[C:44]([CH3:48])[CH:45]=[CH:46][CH:47]=3)=[CH:21][C:22]3[C:23](=[CH:35][CH:36]=[CH:37][CH:38]=3)[C:24]2=[O:25])=[CH:33][CH:32]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 7435Benzoic acid, 3-methyl-, methyl esterHCID 7912DiisopropylamineHCID 8354792-methyl-N-[(4-methylphenyl)methyl]benzamideHCID 2724682Lithium diisopropylamideHCID 178418339Butyllithium

生成物 1

HCID 668834232-(4-methylbenzyl)-3-m-tolyl-2H-isoquinolin-1-one収率 47%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒3 回HCID 8058Hexane溶媒

反応条件

温度
0 °C

実験手順

To a solution of diisopropylamine (1.2 mL, 8.56 mmol) in THF (15 mL) at 0° C. was added n-butyllithium (5.2 mL of a 1.6 M solution in hexane, 8.32 mmol). After stirring at 0° C. for 10 minutes the resulting lithium diisopropylamide solution was treated with a solution of 2-methyl-N-(4-methylbenzyl)benzamide (616 mg, 2.57 mmol) in THF (20 mL) over 15 min. The resulting deep brown-red solution was stirred at 0° C. for 55 minutes at which time it was treated with a solution of 3-methylbenzoic acid methyl ester (0.39 mL, 2.76 mmol) in THF (20 mL) over 20 minutes. After an additional 1 hour at 0° C. the reaction was quenched by the addition of 3N HCl (25 mL). The biphasic mixture was then heated to reflux with vigorous stirring. After 75 minutes at reflux the reaction mixture was allowed to cool to ambient temperature overnight. After cooling overnight, the reaction was concentrated to remove most of the THF. The resulting residue was diluted with ether (100 mL), and water (50 mL), and then basified by careful addition of solid Na2CO3. The basic aqueous was extracted with ether (3×40 mL), combined organics were washed with brine (50 mL), dried over Na2CO3, filtered, and concentrated to afford a yellow oil. The crude product was purified by silica gel column chromatography on a Jones Flashmaster instrument eluting with a gradient from 0% to 6% ethyl acetate/hexane on a 50 g silica column. The product peak was collected to afford 2-(4-methylbenzyl)-3-m-tolyl-2H-isoquinolin-1-one (408 mg, 47% yield) as a yellow oil that slowly solidified to a waxy solid:

後処理

  1. customAfter an additional 1 hour at 0° C. the reaction was quenched by the addition of 3N HCl (25 mL)
  2. temperatureThe biphasic mixture was then heated
  3. temperatureto reflux with vigorous stirring
  4. temperatureAfter 75 minutes at reflux the reaction mixture
  5. temperatureto cool to ambient temperature overnight
  6. temperatureAfter cooling overnight
  7. concentrationthe reaction was concentrated
  8. customto remove most of the THF
  9. additionThe resulting residue was diluted with ether (100 mL), and water (50 mL)
  10. additionbasified by careful addition of solid Na2CO3
  11. extractionThe basic aqueous was extracted with ether (3×40 mL)
  12. washcombined organics were washed with brine (50 mL)
  13. dry with materialdried over Na2CO3
  14. filtrationfiltered
  15. concentrationconcentrated
  16. customto afford a yellow oil
  17. customThe crude product was purified by silica gel column chromatography on a Jones Flashmaster instrument
  18. washeluting with a gradient from 0% to 6% ethyl acetate/hexane on a 50 g silica column
  19. customThe product peak was collected

出典と根拠

ORDレコード
ord-f5d76938870648e28a222f32d13ee019
出典データセット
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07265131B2

反応ノート

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