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Cesium carbonate → N-(4-(4-chloro-2-fluorophenyl)-5-formylpyridin-2-yl)acetamide

HRID 1398352
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HRID 1398352 반응식
Cl[C:2]1[C:7]([CH:8]=[O:9])=[CH:6][N:5]=[C:4]([NH:10][C:11](=[O:13])[CH3:12])[CH:3]=1.[Cl:14][C:15]1[CH:20]=[CH:19][C:18](B(O)O)=[C:17]([F:24])[CH:16]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>O.C1COCC1.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>[Cl:14][C:15]1[CH:20]=[CH:19][C:18]([C:2]2[C:7]([CH:8]=[O:9])=[CH:6][N:5]=[C:4]([NH:10][C:11](=[O:13])[CH3:12])[CH:3]=2)=[C:17]([F:24])[CH:16]=1
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7

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HCID 10796Cesium carbonateHCID 4193595(4-Chloro-2-fluorophenyl)boronic acidHCID 86695931N-(4-chloro-5-formylpyridin-2-yl)acetamide

생성물 1

HCID 86695932N-(4-(4-chloro-2-fluorophenyl)-5-formylpyridin-2-yl)acetamide수율 60%

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매
HCID 962Water용매2회
HCID 8028Tetrahydrofuran용매

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온도
85 °C

실험 절차

To a stirred solution of N-(4-chloro-5-formylpyridin-2-yl)acetamide (3 g, 15.11 mmol), (4-chloro-2-fluorophenyl)boronic acid (2.63 g, 15.11 mmol), cesium carbonate (9.84 g, 30.2 mmol) in a mixture of water (8 mL) and THF (25 mL) was added tetrakis(triphenylphosphine)palladium (19.19 mg, 0.017 mmol) and the reaction was heated to 85° C. overnight (14 h). The reaction mixture was diluted with water (25 mL) and extracted with EtOAc (2×25 mL). The combined organic layers were washed with water (25 mL), brine (25 mL), dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel chromatography (hexane/EtOAc as eluant), yielding N-(4-(4-chloro-2-fluorophenyl)-5-formylpyridin-2-yl)acetamide as an off-white solid (2.8 g, 9.01 mmol, 60% yield). LC/MS (ESI) m/e 291.0 [(M)−, calcd for C14H9ClFN2O2 291.0], LC/MS retention time (method A): tR=1.69 min; 1H NMR (400 MHz, DMSO-d6) δ 11.14 (s, 1H), 9.84 (d, J=Hz, 1H), 8.88 (s, 1H), 8.13 (s, 1H), 7.61 (dd, J=2.00, 10.00 Hz, 1H), 7.46-7.48 (m, 2H), 2.11 (s, 3H).

후처리

  1. extractionextracted with EtOAc (2×25 mL)
  2. washThe combined organic layers were washed with water (25 mL), brine (25 mL)
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel chromatography (hexane/EtOAc as eluant)

출처 및 근거

ORD 기록
ord-11c410e04ea8462cb8590a168f9dccaa
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08901305B2

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