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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → Methyl 2-chloro-2'-(trifluoromethyl)biphenyl-4-carboxylate

HRID 2404335
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HRID 2404335 반응식
B([C:4]1[CH:13]=[CH:12][C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][C:5]=1[Cl:14])(O)O.Br[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[C:22]([F:25])([F:24])[F:23].[F-].[Cs+].O>O1CCOCC1.CC(OC)(C)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>[Cl:14][C:5]1[CH:6]=[C:7]([C:8]([O:10][CH3:11])=[O:9])[CH:12]=[CH:13][C:4]=1[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[C:22]([F:25])([F:24])[F:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 962WaterHCID 9806Benzene, 1-bromo-2-(trifluoromethyl)-HCID 25953Cesium fluorideHCID 221712912-Chloro-4-(methoxycarbonyl)benzeneboronic acid

생성물 1

HCID 66718347Methyl 2-chloro-2'-(trifluoromethyl)biphenyl-4-carboxylate

시약·촉매·용매 3

HCID 178418476
HCID 178418476, 화합물
촉매
HCID 15413tert-Butyl methyl ether용매
HCID 312751,4-Dioxane용매

실험 절차

A mixture of methyl 4-borono-3-chlorobenzoate (Combi-Blocks BB-3530, 1.5 g, 7.0 mmol), 2-bromobenzotrifluoride (1.9 g, 8.4 mmol), cesium fluoride (3.2 g; 21.0 mmol) and bis(triphenylphosphine)palladium(II) chloride (98 mg, 0.14 mmol) was prepared in dioxane (15 mL) and water (7.5 mL) under nitrogen atmosphere, and then heated at 90° C. for 30 minutes. The reaction mixture was diluted with MTBE (30 mL) and washed with water and brine. The aqueous layers were extracted with MTBE (30 mL). The combined organic layers were dried (MgSO4) and concentrated under vacuum. After two purifications by flash chromatography (silica, heptane/DCM, then heptane/EtOAc), the title compound was obtained as a yellow oil. HPLC (Method A) Rt 5.3 min (Purity: 99.7%).

후처리

  1. washwashed with water and brine
  2. extractionThe aqueous layers were extracted with MTBE (30 mL)
  3. dry with materialThe combined organic layers were dried (MgSO4)
  4. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-33f9a1668d9d4ee08d656e807ae48687
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08802704B2

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