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

Potassium Carbonate → HCID 67312595, 화합물

HRID 2190387
노트
인쇄 미리보기

반응식

HRID 2190387 반응식
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[F:11].[C:12]([C:14]([C:17]1[CH:18]=[C:19]([CH:31]=[CH:32][CH:33]=1)[C:20]([NH:22][C:23]1[CH:28]=[C:27]([OH:29])[CH:26]=[CH:25][C:24]=1C)=[O:21])([CH3:16])[CH3:15])#[N:13].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[C:12]([C:14]([C:17]1[CH:18]=[C:19]([CH:31]=[CH:32][CH:33]=1)[C:20]([NH:22][C:23]1[CH:24]=[CH:25][CH:26]=[C:27]([O:29][C:2]2[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=2[F:11])[CH:28]=1)=[O:21])([CH3:16])[CH3:15])#[N:13]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 1230531,2-Difluoro-4-nitrobenzeneHCID 673120273-(1-cyano-1-methylethyl)-N-(5-hydroxy-2-methylphenyl)benzamide

생성물 1

HCID 67312595HCID 67312595, 화합물수율 70%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

To a solution of 1,2-difluoro-4-nitrobenzene (1.19 g, 7.49 mmol) and 3-(1-cyano-1-methylethyl)-N-(5-hydroxy-2-methylphenyl)benzamide (2.0 g, 7.13 mmol) in N,N-dimethylformamide (15 mL) was added potassium carbonate (1.47 g, 10.7 mmol), and the mixture was stirred at 80° C. for 18 hr. The reaction mixture was cooled to room temperature, and concentrated under reduced pressure. The obtained residue was diluted with ethyl acetate (200 mL), washed with water (200 mL) and saturated brine (200 mL), successively, and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=95/5→0/30), and the obtained solution was concentrated under reduced pressure to give the title compound (2.09 g, 70%) as a yellow oil.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. concentrationconcentrated under reduced pressure
  3. additionThe obtained residue was diluted with ethyl acetate (200 mL)
  4. washwashed with water (200 mL) and saturated brine (200 mL)
  5. dry with materialsuccessively, and dried over anhydrous sodium sulfate
  6. filtrationThe insoluble material was filtered off
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=95/5→0/30)
  9. concentrationthe obtained solution was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-dd197970bb9a46768ba55ff126ddd73b
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08324395B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트