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Tetrabutylammonium Fluoride → 3-Ethyl-2-methylpyridine

HRID 31675
ノート
印刷プレビュー

反応式

HRID 31675 の反応式
[CH3:1][C:2]1[C:7]([C:8]#[C:9][Si](C)(C)C)=[CH:6][CH:5]=[CH:4][N:3]=1.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>O1CCCC1>[CH2:8]([C:7]1[C:2]([CH3:1])=[N:3][CH:4]=[CH:5][CH:6]=1)[CH3:9]
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 2724141Tetrabutylammonium FluorideHCID 597925602-Methyl-3-((trimethylsilyl)ethynyl)pyridine

生成物 1

HCID 340873-Ethyl-2-methylpyridine収率 51.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

First, 2-methyl-3-((trimethylsilyl)ethynyl)pyridine (22.6 g, 119 mmol) was dissolved in tetrahydrofuran (dehydrated)(200 ml). To the mixture, tetrabutyl ammonium fluoride (1N tetrahydrofuran solution) (150 ml, 150 mmol) was added. The mixture was stirred at room temperature for one hour. The reaction mixture was partitioned by ethyl acetate and a saturated aqueous ammonium chloride solution. The aqueous layer was extracted with ethyl acetate. The organic layers were combined and washed twice with a saturated aqueous ammonium chloride solution, dried over anhydrous magnesium sulfate, and distilled by a rotary evaporator. To the obtained fraction, 10% palladium/carbon (900 mg) was added and stirred in a hydrogen atmosphere at room temperature for 2 hours. The reaction mixture was filtrated through anhydrous magnesium sulfate and cerite. To the filtrate, 10% palladium/carbon (810 mg) was added and the mixture was stirred in a hydrogen atmosphere at room temperature for 4 hours. The reaction mixture was filtrated through anhydrous magnesium sulfate and celite and thereafter the filtrate was concentrated to obtain the title compound (7.25 g, yield: 51.1%) as a colorless oil.

後処理

  1. customThe reaction mixture was partitioned by ethyl acetate
  2. extractionThe aqueous layer was extracted with ethyl acetate
  3. washwashed twice with a saturated aqueous ammonium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationdistilled by a rotary evaporator
  6. additionTo the obtained fraction, 10% palladium/carbon (900 mg) was added
  7. stirringstirred in a hydrogen atmosphere at room temperature for 2 hours
  8. filtrationThe reaction mixture was filtrated through anhydrous magnesium sulfate
  9. additionTo the filtrate, 10% palladium/carbon (810 mg) was added
  10. stirringthe mixture was stirred in a hydrogen atmosphere at room temperature for 4 hours
  11. filtrationThe reaction mixture was filtrated through anhydrous magnesium sulfate and celite
  12. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-cbbb0be233c548c5ad7914b09060182a
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07425634B2

反応ノート

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