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(4-Chloro-phenyl)-(6-chloro-pyrazin-2-yl)-carbamic acid tert-butyl ester → (4-Chloro-phenyl)-[6-(6-methyl-pyridin-2-yl)-pyrazin-2-yl]-carbamic acid tert-butyl ester

HRID 1961704
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반응식

HRID 1961704 반응식
[Br-].[CH3:2][C:3]1[N:8]=[C:7]([Zn+])[CH:6]=[CH:5][CH:4]=1.[C:10]([O:14][C:15](=[O:31])[N:16]([C:24]1[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][CH:25]=1)[C:17]1[CH:22]=[N:21][CH:20]=[C:19](Cl)[N:18]=1)([CH3:13])([CH3:12])[CH3:11]>O1CCCC1.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>[C:10]([O:14][C:15](=[O:31])[N:16]([C:24]1[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][CH:25]=1)[C:17]1[CH:22]=[N:21][CH:20]=[C:19]([C:7]2[CH:6]=[CH:5][CH:4]=[C:3]([CH3:2])[N:8]=2)[N:18]=1)([CH3:13])([CH3:12])[CH3:11]
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참가 물질

5

반응물 2

HCID 59570677(4-Chloro-phenyl)-(6-chloro-pyrazin-2-yl)-carbamic acid tert-butyl esterHCID 178426002HCID 178426002, 화합물

생성물 1

HCID 59570656(4-Chloro-phenyl)-[6-(6-methyl-pyridin-2-yl)-pyrazin-2-yl]-carbamic acid tert-butyl ester수율 37.5%

시약·촉매·용매 2

HCID 178418476HCID 178418476, 화합물촉매HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

Bis(triphenylphosphine)palladium(II) dichloride (54 mg, 0.076 mmol) was dissolved in degassed tetrahydrofuran (5 mL) Diisobutylaluminum hydride (1M in hexanes, 0.15 mL, 0.15 mmol) was added and the mixture was stirred for 15 minutes. 6-Methyl-2-pyridylzinc bromide (0.5 M in tetrahydrofuran, 2.29 mL, 1.15 mmol) and a solution of (4-chloro-phenyl)-(6-chloro-pyrazin-2-yl)-carbamic acid tert-butyl ester (260 mg, 0.76 mmol) in tetrahydrofuran (3 mL) was added and the mixture was stirred at room temperature over night. The reaction was quenched with aqueous sodium hydrogen carbonate. The aqueous phase was extracted with ethyl acetate (4×15 mL). The combined organic phases were washed with brine, dried over anhydrous sodium sulphate, filtrated and evaporated. The crude product was purified by column chromatography (ethyl acetate/heptane as eluent) to give (4-chloro-phenyl)-[6-(6-methyl-pyridin-2-yl)-pyrazin-2-yl]-carbamic acid tert-butyl ester (113 mg, 23%) as a yellow solid.

후처리

  1. additionwas added
  2. stirringthe mixture was stirred at room temperature over night
  3. customThe reaction was quenched with aqueous sodium hydrogen carbonate
  4. extractionThe aqueous phase was extracted with ethyl acetate (4×15 mL)
  5. washThe combined organic phases were washed with brine
  6. dry with materialdried over anhydrous sodium sulphate
  7. filtrationfiltrated
  8. customevaporated
  9. customThe crude product was purified by column chromatography (ethyl acetate/heptane as eluent)

출처 및 근거

ORD 기록
ord-ced20d67e8394d0db55f3978fc8ef0f3
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08415358B2

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