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1,3,4-Trimethylpyridin-1-ium iodide → 2-Benzyl-1,3,4-trimethyl-1,2-dihydropyridine

HRID 1707599
ノート
印刷プレビュー

反応式

HRID 1707599 の反応式
[CH2:1]([Mg]Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[I-].[CH3:11][N+:12]1[CH:17]=[CH:16][C:15]([CH3:18])=[C:14]([CH3:19])[CH:13]=1>C1COCC1>[CH2:1]([CH:13]1[C:14]([CH3:19])=[C:15]([CH3:18])[CH:16]=[CH:17][N:12]1[CH3:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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 125431661,3,4-Trimethylpyridin-1-ium iodideHCID 178418336HCID 178418336、化合物

生成物 1

HCID 157330592-Benzyl-1,3,4-trimethyl-1,2-dihydropyridine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 3.02M of benzylmagnesium chloride (2M solution) in THF was added portionwise 300 g (20 g portions) of 1,3,4-trimethylpyridinium iodide. The reaction mixture was stirred at room temperature for 18 hrs. The THF was evaporated at reduced pressure, and the resulting residue was poured into iced saturated NH4Cl. The mixture was extracted with ether and the ether solution washed with additional saturated NH4Cl. The ether solution was dried over magnesium sulfate and evaporated to dryness at reduced pressure to afford 338 g of crude 2-benzyl-1,3,4-trimethyl-1,2-dihydropyridine.

後処理

  1. customThe THF was evaporated at reduced pressure
  2. additionthe resulting residue was poured into iced saturated NH4Cl
  3. extractionThe mixture was extracted with ether
  4. washthe ether solution washed with additional saturated NH4Cl
  5. dry with materialThe ether solution was dried over magnesium sulfate
  6. customevaporated to dryness at reduced pressure

出典と根拠

ORDレコード
ord-8af43e54297642a996d015e772d2fe70
出典データセット
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05354758

反応ノート

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