Dimethylcarbamoyl Chloride → 4-Pentyl-2-cyanopyridine

HRID 1269109

反応式

HRID 1269109 の反応式
C[Si]([C:5]#[N:6])(C)C.[CH2:7](OC1C=C[N+]([O-])=CC=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[CH3:22][N:23]([CH3:27])C(Cl)=O.[C:28](=O)(O)[O-].[Na+]>C(Cl)Cl>[CH2:11]([C:10]1[CH:9]=[CH:27][N:23]=[C:22]([C:5]#[N:6])[CH:28]=1)[CH2:12][CH2:13][CH2:8][CH3:7]

参加物

6

反応物 4

HCID 6598Dimethylcarbamoyl ChlorideHCID 82115Trimethylsilyl cyanideHCID 2958714-(Benzyloxy)pyridine N-oxideHCID 516892Sodium Bicarbonate

生成物 1

HCID 210760834-Pentyl-2-cyanopyridine収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To trimethylsilyl cyanide (5.2 g, 52 mmol), 4-benzyloxy-pyridine 1-oxide (8.8 g, 44 mmol) in DCM (20 mL) was added, followed by dimethylcarbamoyl chloride (5.6 g, 52 mmol) in DCM (10 mL), dropwise, stirred at room temperature overnight. Sodium bicarbonate (100 mL, 10%) was added, stirred for 10 minutes and extracted twice with DCM (50 mL). The combined organic layer was dried over magnesium sulfate, solvent was removed to obtain the product, compound 10a (R9=Benzyloxy) (10.5 g, 100%).

後処理

  1. stirringstirred for 10 minutes
  2. extractionextracted twice with DCM (50 mL)
  3. dry with materialThe combined organic layer was dried over magnesium sulfate, solvent
  4. customwas removed

出典と根拠

ORDレコード
ord-070d184ae5474511bc28b7bd985ae504
出典データセット
uspto-grants-2007_04
特許番号
US07199105B2

関連ノート

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