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

3-Carboxyphenylboronic acid → 5'-Fluoro-2'-methoxy-3'-nitro-[1,1'-biphenyl]-3-carboxylic acid

HRID 384293
노트
인쇄 미리보기

반응식

HRID 384293 반응식
Br[C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([N+:9]([O-:11])=[O:10])[C:3]=1[O:12][CH3:13].[C:14]([C:17]1[CH:18]=[C:19](B(O)O)[CH:20]=[CH:21][CH:22]=1)([OH:16])=[O:15]>C(=O)([O-])[O-].[Na+].[Na+].O1CCOCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[F:8][C:6]1[CH:5]=[C:4]([N+:9]([O-:11])=[O:10])[C:3]([O:12][CH3:13])=[C:2]([C:21]2[CH:20]=[CH:19][CH:18]=[C:17]([C:14]([OH:16])=[O:15])[CH:22]=2)[CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 27339573-Carboxyphenylboronic acidHCID 234336121-Bromo-5-fluoro-2-methoxy-3-nitrobenzene

생성물 1

HCID 574837925'-Fluoro-2'-methoxy-3'-nitro-[1,1'-biphenyl]-3-carboxylic acid수율 41.7%

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매HCID 10340Sodium Carbonate
용매
HCID 312751,4-Dioxane용매

반응 조건

온도
120 °C

실험 절차

1-Bromo-5-fluoro-2-methoxy-3-nitro-benzene 2c (16.18 g, 64.7 mmol), 3-carboxyphenylboronic acid (13.88 g, 77.7 mmol) and tetrakis(triphenylphosphine)palladium (3.73 g, 3.2 mmol) were dissolved in the solvent mixture of 65 mL of aqueous sodium carbonate (2 N) and 300 mL of 1,4-dioxane. The reaction mixture was heated to reflux at 120° C. for 24 hours. The reaction was monitored by TLC until the disappearance of the starting materials. The mixture was concentrated under reduced pressure and diluted with 150 mL of hydrochloric acid (6 N) and 200 mL of ethyl acetate. The aqueous layer was extracted with ethyl acetate (100 mL×2). The combined organic extracts were dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to obtain the title compound 5′-fluoro-2′-methoxy-3′-nitro-biphenyl-3-carboxylic acid 2d (7.86 g, yield 41.7%) as a yellow solid.

후처리

  1. temperatureThe reaction mixture was heated
  2. concentrationThe mixture was concentrated under reduced pressure
  3. additiondiluted with 150 mL of hydrochloric acid (6 N) and 200 mL of ethyl acetate
  4. extractionThe aqueous layer was extracted with ethyl acetate (100 mL×2)
  5. dry with materialThe combined organic extracts were dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-3f20d75dba8c4af690d97dc19ae6b4ed
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367710B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트