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

Water → HCID 178487396, 화합물

HRID 2410013
노트
인쇄 미리보기

반응식

HRID 2410013 반응식
[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([C:7]([CH2:18][C:19]3[N:24]=[C:23](/[CH:25]=[CH:26]/[C:27]#[N:28])[CH:22]=[CH:21][CH:20]=3)=[C:8]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[NH:9]2)=[CH:5][CH:4]=1.C(O)(C)C.O.[N-:34]=[N+:35]=[N-:36].[Na+]>Cl.[Br-].[Zn+2].[Br-]>[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([C:7]([CH2:18][C:19]3[CH:20]=[CH:21][CH:22]=[C:23](/[CH:25]=[CH:26]/[C:27]4[NH:36][N:35]=[N:34][N:28]=4)[N:24]=3)=[C:8]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[NH:9]2)=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962Water3회HCID 3776Isopropanol2회HCID 33557Sodium AzideHCID 86703316HCID 86703316, 화합물

생성물 1

HCID 178487396HCID 178487396, 화합물수율 34.5%

시약·촉매·용매 2

HCID 10421208Zinc bromide촉매
HCID 313Hydrochloric Acid용매

실험 절차

To a mixture of (E)-3-[6-(6-methoxy-2-phenyl-1H-indol-3-ylmethyl)pyridin-2-yl]acrylonitrile (67 mg), isopropyl alcohol (1.5 mL) and water (0.5 mL) were added sodium azide (59.6 mg) and zinc bromide (51.6 mg), and the mixture was heated under reflux for 32 hours. Then isopropyl alcohol (1.5 mL) and water (0.5 mL) were added thereto, followed by heating under reflux for 62 hours. The reaction mixture was left to be cooled, diluted with 1 mol/L hydrochloric acid, and then stirred for 5 minutes. To the mixture was added water, followed by extraction with ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluting solvent: ethyl acetate-hexane) to obtain the title compound (25.8 mg). 1H-NMR (DMSO-d6) δ ppm: 3.77 (3H, s), 4.34 (2H, s), 6.65 (1H, dd, J=2.3, 8.5 Hz), 6.87 (1H, d, J=2.3 Hz), 7.16-7.23 (1H, m), 7.32-7.43 (2H, m), 7.46-7.54 (3H, m), 7.65-7.85 (5H, m), 11.16 (1H, s). ESI-MS (m/z): 409 (M+H)+

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 32 hours
  3. temperatureby heating
  4. temperatureunder reflux for 62 hours
  5. waitThe reaction mixture was left
  6. temperatureto be cooled
  7. extractionfollowed by extraction with ethyl acetate
  8. washThe organic layer was washed with water
  9. dry with materialdried over anhydrous magnesium sulfate
  10. concentrationconcentrated under reduced pressure
  11. customThe residue was purified by silica gel column chromatography (eluting solvent: ethyl acetate-hexane)

출처 및 근거

ORD 기록
ord-72c3ee5f65994aada480e5818291c402
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08815903B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트