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tert-Butyl acrylate → (E)-tert-Butyl 3-(1H-pyrrolo[2,3-b]pyridin-5-yl)acrylate t-butyl acrylate

HRID 83027
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HRID 83027 반응식
[C:1]([O:5][C:6]([CH3:9])([CH3:8])[CH3:7])(=[O:4])[CH:2]=[CH2:3].C(N(C(C)C)CC)(C)C.CC1C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.Br[C:42]1[CH:43]=[C:44]2[CH:50]=[CH:49][NH:48][C:45]2=[N:46][CH:47]=1>C(#N)CC.CN(C)C=O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[C:6]([O:5][C:1](=[O:4])[CH:2]=[CH2:3])([CH3:9])([CH3:8])[CH3:7].[NH:48]1[C:45]2=[N:46][CH:47]=[C:42](/[CH:3]=[CH:2]/[C:1]([O:5][C:6]([CH3:9])([CH3:8])[CH3:7])=[O:4])[CH:43]=[C:44]2[CH:50]=[CH:49]1
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8

반응물 4

HCID 15458tert-Butyl acrylateHCID 80271Tri-o-tolylphosphineHCID 81531DiisopropylethylamineHCID 103079325-bromo-1H-pyrrolo[2,3-b]pyridine

생성물 1

HCID 86672984(E)-tert-Butyl 3-(1H-pyrrolo[2,3-b]pyridin-5-yl)acrylate t-butyl acrylate

시약·촉매·용매 3

HCID 167845
palladium(II) acetate
촉매
HCID 6228Dimethylformamide용매
HCID 7854Propionitrile용매

실험 절차

tert-Butyl acrylate (5.9 mL, 40.6 mmol), diisopropylethylamine (3.5 mL, 20.3 mmol) and P(o-tolyl)3 (618 mg, 2.0 mmol) were successively added to a suspension of 5-bromo-1H-pyrrolo[2,3-b]pyridine (2.0 g, 10.15 mmol) in propionitrile (40 mL) and dimethylformamide (10 mL). The resulting mixture was purged with argon prior to the addition of palladium acetate (227 mg, 1.0 mmol). The mixture was then purged with argon a second time and refluxed overnight. The reaction mixture was filtered on Celite®. The filtrate was concentrated to dryness and the residue was solubilized in ethyl acetate (3×100 mL). The organic layers were washed with a saturated solution of sodium chloride (3×50 mL), dried over sodium sulfate, filtered and concentrated to dryness. The crude was purified by flash chromatography on silica gel using dichloromethane/ethyl acetate (1:0 to 7:3) as eluent. The title compound was obtained as a yellow solid (465 mg, 28%)

후처리

  1. customThe resulting mixture was purged with argon
  2. customThe mixture was then purged with argon a second time
  3. temperaturerefluxed overnight
  4. filtrationThe reaction mixture was filtered on Celite®
  5. concentrationThe filtrate was concentrated to dryness
  6. washThe organic layers were washed with a saturated solution of sodium chloride (3×50 mL)
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated to dryness
  10. customThe crude was purified by flash chromatography on silica gel

출처 및 근거

ORD 기록
ord-5c080ca66af54f07991c6dedcba90f0a
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846711B2

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