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

Cesium carbonate → HCID 58046355, 화합물

HRID 2359296
노트
인쇄 미리보기

반응식

HRID 2359296 반응식
[CH2:1]([C:3]1[CH:8]=[C:7]([F:9])[CH:6]=[CH:5][C:4]=1[OH:10])[CH3:2].C(=O)([O-])[O-].[Cs+].[Cs+].[Cl:17][C:18]1[C:19](F)=[CH:20][C:21]([F:27])=[C:22]([CH:26]=1)[C:23]([OH:25])=[O:24]>CS(C)=O>[F:27][C:21]1[CH:20]=[C:19]([O:10][C:4]2[CH:5]=[CH:6][C:7]([F:9])=[CH:8][C:3]=2[CH2:1][CH3:2])[C:18]([Cl:17])=[CH:26][C:22]=1[C:23]([OH:25])=[O:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 27371852-Ethyl-4-fluorophenolHCID 148764175-Chloro-2,4-difluorobenzoic acid

생성물 1

HCID 58046355HCID 58046355, 화합물수율 57.2%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a solution of 2-ethyl-4-fluorophenol (364 mg, 2.60 mmol) in DMSO (10 mL) was added cesium carbonate (1690 mg, 5.19 mmol) and the mixture stirred at room temperature for 5 minutes. 5-chloro-2,4-difluorobenzoic acid (500 mg, 2.6 mmol) was added and the reaction heated to 110° C. for 18 hours. The reaction was cooled and quenched by the addition of 1N HCl (30 mL) and extracted into ethyl acetate (3×30 mL). The organic layers were combined, washed with brine (30 mL) and concentrated in vacuo before purifying using silica gel column chromatography eluting with ethylacetate:heptane 12:88 to 100:0 to furnish the title compound as a white solid (465 mg, 57%).

후처리

  1. temperaturethe reaction heated to 110° C. for 18 hours
  2. temperatureThe reaction was cooled
  3. customquenched by the addition of 1N HCl (30 mL)
  4. extractionextracted into ethyl acetate (3×30 mL)
  5. washwashed with brine (30 mL)
  6. concentrationconcentrated in vacuo
  7. custombefore purifying
  8. washeluting with ethylacetate:heptane 12:88 to 100:0

출처 및 근거

ORD 기록
ord-9a2684c6e0ce4b5fa2800d85dd948a9b
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08685977B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트