Hydrochloric Acid → 2-Methyl-6-(1h-1,2,4-triazol-1-yl)pyridin-3-ol

HRID 1931575

반응식

HRID 1931575 반응식
[CH3:1][C:2]1[C:7]([O:8]C(=O)C)=[CH:6][CH:5]=[C:4]([N:12]2[CH:16]=[N:15][CH:14]=[N:13]2)[N:3]=1.[OH-].[Na+].Cl>>[CH3:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[C:4]([N:12]2[CH:16]=[N:15][CH:14]=[N:13]2)[N:3]=1

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 669152932-Methyl-6-(1H-1,2,4-triazol-1-yl)pyridin-3-yl acetate

생성물 1

HCID 579650072-Methyl-6-(1h-1,2,4-triazol-1-yl)pyridin-3-ol수율 95.6%

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온도
0 °C

실험 절차

Acetic acid 2-methyl-6-[1,2,4]triazol-1-yl-pyridin-3-yl ester (125 mg, 0.57 mmol) was added to 2 M aqueous sodium hydroxide solution (1.6 mL) at 0° C. to give a slurry, and the mixture was stirred at 0° C. for 20 min and then at room temperature for 3 h. 2 M Aqueous hydrochloric acid was added to bring the pH to 6, and the mixture was extracted four times with ethyl acetate. The organic layers were combined and the solvent was evaporated to dryness to give 2-methyl-6-[1,2,4]triazol-1-yl-pyridin-3-ol (96 mg, 95%) as a white powder. 1H NMR (300 MHz, DMSO-d6) δ 2.36 (s, 3H), 7.33 (d, 1H, J=8.7 Hz), 7.51 (d, 1H, J=8.5 Hz), 8.18 (s, 1H), 9.12 (s, 1H), 10.19 (br s, 1H).

후처리

  1. customto give a slurry
  2. waitat room temperature for 3 h
  3. extractionthe mixture was extracted four times with ethyl acetate
  4. customthe solvent was evaporated to dryness

출처 및 근거

ORD 기록
ord-6f5d41db9a914a05b48ac577ec265557
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188098B2

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