Sodium Hydroxide → HCID 86672135, 화합물

HRID 82313

반응식

HRID 82313 반응식
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

참가 물질

5

반응물 2

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

생성물 1

HCID 86672135HCID 86672135, 화합물수율 99%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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]−

후처리

  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

출처 및 근거

ORD 기록
ord-8a7dcd844d9f4a55a6a7deb2c767930a
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846698B2

연결된 노트

불러오는 중…