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

Water → 5-(4-Fluoro-3-formylphenyl)-indazole-1-carboxylic acid tert-butyl ester

HRID 1435558
노트
인쇄 미리보기

반응식

HRID 1435558 반응식
[C:1]([O:5][C:6]([N:8]1[C:16]2[C:11](=[CH:12][C:13](Br)=[CH:14][CH:15]=2)[CH:10]=[N:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[F:18][C:19]1[CH:26]=[C:25](C2OC(C)(C)C(C)(C)O2)[CH:24]=[CH:23][C:20]=1[CH:21]=[O:22].C(Cl)Cl.C(=O)([O-])[O-].[Cs+].[Cs+].O>O1CCOCC1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[C:1]([O:5][C:6]([N:8]1[C:16]2[C:11](=[CH:12][C:13]([C:24]3[CH:25]=[CH:26][C:19]([F:18])=[C:20]([CH:21]=[O:22])[CH:23]=3)=[CH:14][CH:15]=2)[CH:10]=[N:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 962WaterHCID 6344DichloromethaneHCID 10796Cesium carbonateHCID 228320255-Bromo-1H-indazole, N1-BOC protectedHCID 86620564HCID 86620564, 화합물

생성물 1

HCID 866164695-(4-Fluoro-3-formylphenyl)-indazole-1-carboxylic acid tert-butyl ester수율 71.5%

시약·촉매·용매 2

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)촉매HCID 312751,4-Dioxane용매

반응 조건

온도
85 °C

실험 절차

A mixture of 5-bromo-indazole-1-carboxylic acid tert-butyl ester (3.37 mmol), 2-fluoro-4-(4,4,5,5-tetramethyl-[1,3] dioxolan-2-yl)-benzaldehyde (1.01 g, 4.04 mmol)) PdCl2(dppf).DCM (27 mg, 0.03 mmol) in 16 mL of dioxane was degassed (evacuate in vacuo and pressurize with argon, three times); cesium carbonate in water (2M, 6.73 mL, 13.46 mmol) was added and the mixture degassed three more times as described above. The resulting mixture was heated at 85° C. for 6 h, then it was allowed to cool to room temperature and left overnight. The mixture was diluted with dichloromethane and washed with brine. The aqueous phase was extracted with dichloromethane and the combined organic phases were washed with brine, dried over MgSO4, filtered and evaporated to give crude product. Chromatography on silica gel (elution with diethyl ether/heptane) gave 820 mg of the title compound.

후처리

  1. custom(evacuate in vacuo and pressurize with argon, three times)
  2. customthe mixture degassed three more times
  3. temperatureto cool to room temperature
  4. additionThe mixture was diluted with dichloromethane
  5. washwashed with brine
  6. extractionThe aqueous phase was extracted with dichloromethane
  7. washthe combined organic phases were washed with brine
  8. dry with materialdried over MgSO4
  9. filtrationfiltered
  10. customevaporated
  11. customto give crude product

출처 및 근거

ORD 기록
ord-bc21cd5fa5dd467093117d3c4ed36577
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07618650B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트