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

N-(3-{[(7-{[(3-Hydroxyphenyl)amino]sulfonyl}-9-oxo-9H-fluoren-2-yl)sulfonyl]amino}phenyl)acetamide → N-(3-Aminophenyl)-N'-(3-hydroxyphenyl)-9-oxo-9H-fluorene-2,7-disulfonamide

HRID 2120918
노트
인쇄 미리보기

반응식

HRID 2120918 반응식
[OH:1][C:2]1[CH:3]=[C:4]([NH:8][S:9]([C:12]2[CH:24]=[C:23]3[C:15]([C:16]4[CH:17]=[CH:18][C:19]([S:26]([NH:29][C:30]5[CH:31]=[C:32]([NH:36]C(=O)C)[CH:33]=[CH:34][CH:35]=5)(=[O:28])=[O:27])=[CH:20][C:21]=4[C:22]3=[O:25])=[CH:14][CH:13]=2)(=[O:11])=[O:10])[CH:5]=[CH:6][CH:7]=1>C1COCC1.CO.[OH-].[Na+]>[NH2:36][C:32]1[CH:31]=[C:30]([NH:29][S:26]([C:19]2[CH:18]=[CH:17][C:16]3[C:15]4[C:23](=[CH:24][C:12]([S:9]([NH:8][C:4]5[CH:5]=[CH:6][CH:7]=[C:2]([OH:1])[CH:3]=5)(=[O:10])=[O:11])=[CH:13][CH:14]=4)[C:22](=[O:25])[C:21]=3[CH:20]=2)(=[O:27])=[O:28])[CH:35]=[CH:34][CH:33]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 9985345N-(3-{[(7-{[(3-Hydroxyphenyl)amino]sulfonyl}-9-oxo-9H-fluoren-2-yl)sulfonyl]amino}phenyl)acetamide

생성물 1

HCID 10436736N-(3-Aminophenyl)-N'-(3-hydroxyphenyl)-9-oxo-9H-fluorene-2,7-disulfonamide수율 59.5%

시약·촉매·용매 2

HCID 14798Sodium Hydroxide용매HCID 21899815MeOH tetrahydrofuran용매

실험 절차

The product from Example 6A (289 mg, 0.554 mmol) in THF:MeOH (1:1, 20 mL) and 15% aq NaOH (10 mL) was heated at reflux. After 24 hours, the volatiles were evaporated at reduced pressure and the residue was partitioned between ethyl acetate and saturated NaHCO3. The separated aqueous phase was extracted with ethyl acetate. The combined organic extracts were washed with brine, dried (Na2SO4), filtered, and the filtrate concentrated under reduced pressure. The residue was purified by flash chromatography (80% ethyl acetate/hexanes) to provide the title compound as an orange solid (172 mg, 55% yield). 1H NMR (300 MHz, DMSO-d6) δ 9.50 (1H), 7.97-8.1 (m, 4H), 7.92 (d, 2H), 7.00 (t, 1H), 6.83 (t, 1H), 6.58 (t, 1H), 6.53 (m, 1H), 6.42 (m, 1H), 6.35 (t, 1H), 6.22 (m, 2H), 5.14 (bs, 2H). MS (ESI) 520 (M−H)−.

후처리

  1. temperatureat reflux
  2. customthe volatiles were evaporated at reduced pressure
  3. customthe residue was partitioned between ethyl acetate and saturated NaHCO3
  4. extractionThe separated aqueous phase was extracted with ethyl acetate
  5. washThe combined organic extracts were washed with brine
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationthe filtrate concentrated under reduced pressure
  9. customThe residue was purified by flash chromatography (80% ethyl acetate/hexanes)

출처 및 근거

ORD 기록
ord-fefa999b714d4340b3ef7fda282ec6de
출처 데이터셋
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06693136B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트