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

Cesium carbonate → HCID 178497098, 화합물

HRID 931399
노트
인쇄 미리보기

반응식

HRID 931399 반응식
Br[C:2]1[C:3]([NH:9][C:10](=[O:25])[C:11](=[CH2:24])[CH:12]([C:14]2[CH:19]=[CH:18][C:17]([C:20]([O:22][CH3:23])=[O:21])=[CH:16][CH:15]=2)[CH3:13])=[N+:4]([O-:8])[CH:5]=[CH:6][CH:7]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH3:23][O:22][C:20]([C:17]1[CH:16]=[C:15]2[C:14](=[CH:19][CH:18]=1)[CH:12]([CH3:13])[C:11]1([C:2]3[C:3](=[N+:4]([O-:8])[CH:5]=[CH:6][CH:7]=3)[NH:9][C:10]1=[O:25])[CH2:24]2)=[O:21]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 10796Cesium carbonateHCID 178459998HCID 178459998, 화합물

생성물 1

HCID 178497098HCID 178497098, 화합물

시약·촉매·용매 2

HCID 178418476HCID 178418476, 화합물촉매HCID 6228Dimethylformamide용매

반응 조건

온도
110 °C

실험 절차

Bis(triphenylphosphine)palladium(II) dichloride (0.17 g, 0.24 mmol) was added to a deoxygenated mixture of 3-bromo-2-(3-(4-(methoxycarbonyl)phenyl)-2-methylenebutanamido)pyridine 1-oxide (2.0 g, 5.0 mmol), cesium carbonate (4.03 g, 12.4 mmol) in anhydrous DMF (40 mL). The resulting mixture was heated at 110° C. under nitrogen for 20 h, then cooled and filtered through Celite®. The filter cake was washed with ethyl acetate. The filtrate was concentrated, and partitioned between ethyl acetate and brine (2×). The combined organic layers were dried over anhydrous sodium sulfate and concentrated to give the title compound which was used without further purification in next step.

후처리

  1. temperaturecooled
  2. filtrationfiltered through Celite®
  3. washThe filter cake was washed with ethyl acetate
  4. concentrationThe filtrate was concentrated
  5. custompartitioned between ethyl acetate and brine (2×)
  6. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-790f850ee3f84e9fb2f44123c45e04ef
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296750B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트