홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Methane → Lesinurad

HRID 38745
노트
인쇄 미리보기

반응식

HRID 38745 반응식
[OH-:1].[Na+].[Br:3][C:4]1[N:5]([C:25]2[C:34]3[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=3)[C:28]([CH:35]3[CH2:37][CH2:36]3)=[CH:27][CH:26]=2)[C:6]([S:9][CH2:10][C:11](NC2C=CC(S(=O)(=O)N)=CC=2Cl)=[O:12])=[N:7][N:8]=1.C>C(O)C>[Br:3][C:4]1[N:5]([C:25]2[C:34]3[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=3)[C:28]([CH:35]3[CH2:37][CH2:36]3)=[CH:27][CH:26]=2)[C:6]([S:9][CH2:10][C:11]([OH:1])=[O:12])=[N:7][N:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 297MethaneHCID 14798Sodium HydroxideHCID 115199512-(5-bromo-4-(4-cyclopropylnaphthalen-1-yl)-4H-1,2,4-triazol-3-ylthio)-N-(2-chloro-4-sulfamoylphenyl)acetamide

생성물 1

HCID 53465279Lesinurad

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Sodium hydroxide solution (2M aqueous, 33.7 mL, 67 mmol, 2 eq) was added to a suspension of 2-(5-bromo-4-(4-cyclopropylnaphthalen-1-yl)-4H-1,2,4-triazol-3-ylthio)-N-(2-chloro-4-sulfamoylphenyl)acetamide (prepared by previously published procedures, see US 2009/0197825; 20 g, 34 mmol) in ethanol (200 mL) and the mixture heated at reflux for 4 hours. Charcoal (10 g) was added, the mixture stirred at room temperature for 12 hours and the charcoal removed by filtration. The charcoal was washed several times with ethanol and the filtrate then concentrated. Water (200 mL) was added and then concentrated to approx. one third volume to remove all ethanol. Water (200 mL) and ethyl acetate (250 mL) were added, the mixture stirred vigorously for 15 min and the organic layer removed. The aqueous layer was cooled to 0° C. and acidified by treatment with HCl (1N) resulting in the formation of a cloudy oily precipitate. The mixture was extracted with ethyl acetate (3×) and the combined organic extracts dried over sodium sulfate and concentrated to give 2-(5-bromo-4-(4-cyclopropylnaphthalen-1-yl)-4H-1,2,4-triazol-3-ylthio)acetic acid as an off white solid (11.2 g, 82%).

후처리

  1. customprepared by previously published procedures
  2. temperatureat reflux for 4 hours
  3. customthe charcoal removed by filtration
  4. washThe charcoal was washed several times with ethanol
  5. concentrationthe filtrate then concentrated
  6. additionWater (200 mL) was added
  7. concentrationconcentrated
  8. customto remove all ethanol
  9. additionWater (200 mL) and ethyl acetate (250 mL) were added
  10. stirringthe mixture stirred vigorously for 15 min
  11. customthe organic layer removed
  12. temperatureThe aqueous layer was cooled to 0° C.
  13. customresulting in the formation of a cloudy oily precipitate
  14. extractionThe mixture was extracted with ethyl acetate (3×)
  15. dry with materialthe combined organic extracts dried over sodium sulfate
  16. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3bf07a84810d4d41aa162f2a8e296ede
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08524754B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트