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

HRID 1931575

反応式

HRID 1931575 の反応式
[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

参加物

4

反応物 3

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

生成物 1

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

反応条件

温度
0 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-6f5d41db9a914a05b48ac577ec265557
出典データセット
uspto-grants-2012_05
特許番号
US08188098B2

関連ノート

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