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Diethyl Ether → 5-Bromo-4-methylpyridine-3-carbaldehyde

HRID 1909011
ノート
印刷プレビュー

反応式

HRID 1909011 の反応式
Br[C:2]1[CH:7]=C[CH:5]=[C:4]([Br:8])[C:3]=1[CH3:9].CC[O:12]CC.[Li]CCCC.[CH3:20][N:21](C=O)C>C1COCC1>[Br:8][C:4]1[C:3]([CH3:9])=[C:2]([CH:7]=[O:12])[CH:20]=[N:21][CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 6228DimethylformamideHCID 346812,6-DibromotolueneHCID 178418339Butyllithium

生成物 1

HCID 222383375-Bromo-4-methylpyridine-3-carbaldehyde

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

2,6-Dibromotoluene (9.8 g, 39 mmol) in THF (300 mL) was stirred under N2 and was then cooled to −100° C. (ether/liquid N2). n-BuLi (16.4 mL, 41 mmol, 2.5 M in hexane) was then added drop wise and after stirring for 5 minutes DMF (4.5 mL, 58.6 mmol) was added. The reaction was stirred for a further 20 minutes and then for an hour at −78° C. The reaction was quenched with saturated aqueous NH4Cl and allowed to warm up to room temperature. The reaction was diluted with water and the pH adjusted to pH 7-8 with sat. aqueous NaHCO3. The mixture was evaporated in vacuo to remove the THF, and the product was then extracted with Et2O (×3). The combined organic layers were washed with brine and dried (MgSO4). The product was filtered and evaporated on vacuo to give 5-bromo-4-methyl-pyridine-3-carbaldehyde as a colourless solid which was used without further purification.

後処理

  1. additionwas added
  2. waitfor an hour at −78° C
  3. customThe reaction was quenched with saturated aqueous NH4Cl
  4. additionThe reaction was diluted with water
  5. customThe mixture was evaporated in vacuo
  6. customto remove the THF
  7. extractionthe product was then extracted with Et2O (×3)
  8. washThe combined organic layers were washed with brine
  9. dry with materialdried (MgSO4)
  10. filtrationThe product was filtered
  11. customevaporated on vacuo

出典と根拠

ORDレコード
ord-1ad73e2380ac4b4fb4dc041d0f44672f
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08598217B2

反応ノート

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