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Sodium hydride → 6-bromo-3-methyl-2,3-dihydro-1H-indol-2-one

HRID 878986
ノート
印刷プレビュー

反応式

HRID 878986 の反応式
[H-].[Na+].C[CH2:4][CH:5](C(OCC)=O)[C:6](OC)=[O:7].Br[C:16]1[CH:21]=[CH:20][C:19]([Br:22])=[CH:18][C:17]=1[N+:23]([O-])=O>CS(C)=O>[Br:22][C:19]1[CH:18]=[C:17]2[C:16]([CH:5]([CH3:4])[C:6](=[O:7])[NH:23]2)=[CH:21][CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 770041,4-Dibromo-2-nitrobenzeneHCID 5088009HCID 5088009、化合物

生成物 1

HCID 2803186-bromo-3-methyl-2,3-dihydro-1H-indol-2-one

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒2 回

実験手順

Sodium hydride (3.9 g) was suspended in dimethyl sulfoxide (24 mL), and diethyl methyl malonate (16 mL) was added at 0° C., and then the reaction mixture was stirred at room temperature for 1.5 hours. The reaction mixture was heated to 100° C., and a solution of 2,5-dibromonitrobenzene (15.3 g) in dimethyl sulfoxide (17 mL) was added at 100° C., and then the reaction mixture was stirred at 100° C. for 5 hours. The reaction mixture was quenched with water, and extracted with ethyl acetate. The obtained organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated under reduced pressure. The residue was dissolved in ethanol (75 mL), and tin (11.5 g) was added at room temperature. Concentrated hydrochloric acid (45 mL) was added at 0° C., and then the reaction mixture was heated at reflux for 2 hours. After cooling to room temperature, the reaction mixture was quenched with water, and extracted with ethyl acetate. The obtained organic layer was washed with a saturated aqueous solution of sodium hydrogen carbonate and brine, dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography to give the titled compound (4.9 g) as a brown solid.

後処理

  1. temperatureThe reaction mixture was heated to 100° C.
  2. stirringthe reaction mixture was stirred at 100° C. for 5 hours
  3. customThe reaction mixture was quenched with water
  4. extractionextracted with ethyl acetate
  5. washThe obtained organic layer was washed with brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationthe filtrate was concentrated under reduced pressure
  9. dissolutionThe residue was dissolved in ethanol (75 mL)
  10. additiontin (11.5 g) was added at room temperature
  11. additionConcentrated hydrochloric acid (45 mL) was added at 0° C.
  12. temperaturethe reaction mixture was heated
  13. temperatureat reflux for 2 hours
  14. temperatureAfter cooling to room temperature
  15. customthe reaction mixture was quenched with water
  16. extractionextracted with ethyl acetate
  17. washThe obtained organic layer was washed with a saturated aqueous solution of sodium hydrogen carbonate and brine
  18. dry with materialdried over anhydrous sodium sulfate
  19. filtrationfiltered
  20. concentrationthe filtrate was concentrated under reduced pressure
  21. customThe obtained residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-4ba37a4ae37e4a4da984e4c816e3f034
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08987473B2

反応ノート

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