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

HRID 1640108

반응식

HRID 1640108 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f5ff02d794014095bf81206b1d4540ab
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08110687B2

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