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Cesium carbonate → 4-Fluoro-1-(3-nitro-5-(trifluoromethyl)phenyl)piperidine

HRID 2200144
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HRID 2200144 반응식
Br[C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([N+:12]([O-:14])=[O:13])[CH:3]=1.Cl.[F:16][CH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.C(=O)([O-])[O-].[Cs+].[Cs+]>O1CCOCC1.O.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(P(C2C=CC=CC=2)C2C=CC3C(=CC=CC=3)C=2C2C3C(=CC=CC=3)C=CC=2P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[F:16][CH:17]1[CH2:22][CH2:21][N:20]([C:2]2[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([N+:12]([O-:14])=[O:13])[CH:3]=2)[CH2:19][CH2:18]1
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참가 물질

8

반응물 3

HCID 10796Cesium carbonateHCID 27591584-Fluoropiperidine hydrochlorideHCID 70154111-Bromo-3-nitro-5-(trifluoromethyl)benzene

생성물 1

HCID 900206124-Fluoro-1-(3-nitro-5-(trifluoromethyl)phenyl)piperidine수율 63.4%

시약·촉매·용매 4

HCID 634876Binap, (A+-)-촉매
HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 962Water용매
HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

Mix 1-bromo-3-nitro-5-(trifluoromethyl)benzene (700 mg, 2.59 mmol), 4-fluoropiperidine hydrochloride (544 mg, 3.89 mmol), cesium carbonate (2.5 g, 7.77 mmol), (±)-2,2′-bis(diphenylphosphino)-1,1′-binaphthalene (BINAP, 48 mg, 0.077 mmol), tris(dibenzylideneacetone)dipalladium [Pd2(dba)3, 47 mg, 0.052 mmol] in dioxane (10 mL), Stir the mixture under nitrogen atmosphere at 100° C. for 16 hrs. Cool the reaction mixture to room temperature, dilute it with water (10 mL), extract with ethyl acetate (10 mL×2), combine the organic layers, wash with brine (15 mL) and dry over anhydrous sodium sulfate. Concentrate the filtrate to get the crude product. Purify by flash chromatography (silica gel, 100% PE) to yield the target compound (480 mg, 63%).

후처리

  1. temperatureCool the reaction mixture to room temperature
  2. extractionextract with ethyl acetate (10 mL×2)
  3. washwash with brine (15 mL)
  4. dry with materialdry over anhydrous sodium sulfate
  5. concentrationConcentrate the filtrate
  6. customto get the crude product
  7. customPurify by flash chromatography (silica gel, 100% PE)

출처 및 근거

ORD 기록
ord-ad5bb0cf52584ba09693fc092e428a39
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09359338B2

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