Potassium Carbonate → 4-nitro-2-(1H-1,2,4-triazol-1-yl)pyridine 1-oxide

HRID 1640108

反応式

HRID 1640108 の反応式
Cl[C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][N+:3]=1[O-:11].C[Si](C)(C)[N:14]1[CH:18]=[N:17][CH:16]=[N:15]1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[N+:8]([C:6]1[CH:5]=[CH:4][N+:3]([O-:11])=[C:2]([N:14]2[CH:18]=[N:17][CH:16]=[N:15]2)[CH:7]=1)([O-:10])=[O:9]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 844332-Chloro-4-nitropyridine 1-oxideHCID 875581-Trimethylsilyl-1,2,4-triazole

生成物 1

HCID 667213864-nitro-2-(1H-1,2,4-triazol-1-yl)pyridine 1-oxide収率 27.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2-chloro-4-nitropyridine 1-oxide (2.00 g, 11.4 mmol) and 1-(trimethylsilyl)-1H-1,2,4-triazole (1.64 mL, 11.4 mmol) in DMF (40 mL), was added potassium carbonate (4.75 g, 34.4 mmol). The reaction mixture was allowed to stir at rt for 2 h. The DMF was evaporated and water was added. The precipitate was filtered and washed with water then hexane and dried under vacuum. The solid was purified by column to give 4-nitro-2-(1H-1,2,4-triazol-1-yl)pyridine 1-oxide (0.643 g, 27.1%) as a pale yellow solid. LCMS: (FA) ES+ 208.1, ES− 206.1.

後処理

  1. customThe DMF was evaporated
  2. additionwater was added
  3. filtrationThe precipitate was filtered
  4. washwashed with water
  5. dry with materialhexane and dried under vacuum
  6. customThe solid was purified by column

出典と根拠

ORDレコード
ord-f5ff02d794014095bf81206b1d4540ab
出典データセット
uspto-grants-2012_02
特許番号
US08110687B2

関連ノート

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