Sodium Hydroxide → HCID 86672135、化合物

HRID 82313

反応式

HRID 82313 の反応式
C([O:3][C:4](=[O:18])[CH2:5][N:6]1[CH:10]=[C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([OH:17])[CH:12]=2)[N:8]=[N:7]1)C.[OH-].[Na+]>CO.O>[OH2:3].[OH:17][C:13]1[CH:12]=[C:11]([C:9]2[N:8]=[N:7][N:6]([CH2:5][C:4]([OH:18])=[O:3])[CH:10]=2)[CH:16]=[CH:15][CH:14]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 70847799Ethyl[4-(3-Hydroxyphenyl)-1H-1,2,3-triazol-1-yl]acetate

生成物 1

HCID 86672135HCID 86672135、化合物収率 99%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

Ethyl[4-(3-Hydroxyphenyl)-1H-1,2,3-triazol-1-yl]acetate (Preparation 291, 27.2 g, 0.110 mol) was dissolved in methanol (200 mL), and a solution of NaOH (4.84 g, 121 mmol) in water (40 mL) was added. The solution was kept at room temperature for 24 hours. Methanol was evaporated in vacuo, water (120 mL) was added, and the solution was refluxed with activated charcoal. The mixture was filtered, and 11 M HCl was added to the filtrate. The mixture was dissolved by addition of water (120 mL) and cooled to carry out the crystallization. The crystals were filtered, washed with water (2×25 mL), and evaporated to dryness to afford the title compound as brown crystals (mp 186.3-188.7° C.) in 99.0% yield 23.9 g. MS m/z 218 [M−H]−

後処理

  1. customMethanol was evaporated in vacuo, water (120 mL)
  2. additionwas added
  3. temperaturethe solution was refluxed with activated charcoal
  4. filtrationThe mixture was filtered
  5. addition11 M HCl was added to the filtrate
  6. dissolutionThe mixture was dissolved by addition of water (120 mL)
  7. temperaturecooled
  8. customthe crystallization
  9. filtrationThe crystals were filtered
  10. washwashed with water (2×25 mL)
  11. customevaporated to dryness

出典と根拠

ORDレコード
ord-8a7dcd844d9f4a55a6a7deb2c767930a
出典データセット
uspto-grants-2014_09
特許番号
US08846698B2

関連ノート

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