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1,1'-Carbonyldiimidazole → tert-Butyl 1-(3,5-dibromopyrazin-2-ylamino)-2-methyl-1-oxopropan-2-ylcarbamate

HRID 717123
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Reaktionsgleichung

Reaktionsgleichung von HRID 717123
C(N1C=CN=C1)(N1C=CN=C1)=O.[C:13]([O:17][C:18]([NH:20][C:21]([CH3:26])([CH3:25])[C:22]([OH:24])=O)=[O:19])([CH3:16])([CH3:15])[CH3:14].C(N(CC)C(C)C)(C)C.[Br:36][C:37]1[C:38]([NH2:44])=[N:39][CH:40]=[C:41]([Br:43])[N:42]=1>CN(C)C=O.ClCCl>[Br:36][C:37]1[C:38]([NH:44][C:22](=[O:24])[C:21]([NH:20][C:18](=[O:19])[O:17][C:13]([CH3:14])([CH3:15])[CH3:16])([CH3:26])[CH3:25])=[N:39][CH:40]=[C:41]([Br:43])[N:42]=1
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Komponenten

7

Edukt 4

HCID 682631,1'-CarbonyldiimidazoleHCID 81531DiisopropylethylamineHCID 6200042-Amino-3,5-dibromopyrazineHCID 2733845N-((1,1-dimethylethoxy)carbonyl)-2-methyl-alanine

Produkt 1

HCID 86696610tert-Butyl 1-(3,5-dibromopyrazin-2-ylamino)-2-methyl-1-oxopropan-2-ylcarbamateAusbeute 37 %

Reagenzien, Katalysatoren, Lösungsmittel

2
HCID 6228DimethylformamideLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

1,1′-Carbonyldiimidazole (2.63 g, 16.24 mmol) was added to a stirred solution of 2-(tert-butoxycarbonylamino)-2-methylpropanoic acid (3.00 g, 14.76 mmol) in N,N-dimethylformamide (4 mL) and dichloromethane (8 mL) at room temperature. The resulting clear colorless mixture was stirred at room temperature under nitrogen for 3 h. N,N-Diisopropylethylamine (3.86 mL, 22.14 mmol) was added followed by 3,5-dibromopyrazin-2-amine (5.60 g, 22.14 mmol). The resulting mixture was heated at 50° C. under a reflux condenser under nitrogen for 71 h. Dichloromethane was removed under reduced pressure. The residue was diluted with ethyl acetate and washed with water. The water layer was extracted with ethyl acetate. The combined organics were washed with brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue was triturated with 30% ethyl acetate in hexane and solids collected by vacuum filtration. The filtrate was concentrated under reduced pressure and purified using flash chromatography (5-50% ethyl acetate in hexane). Fractions containing the desired product were combined with the solids obtained by filtration and concentrated under reduced pressure. The residue was dried under high vacuum to give the desired product (2.38 g, 5.43 mmol, 37% yield) as an off-white solid. MS (ESI) m/z 439.3 [M+1]+, 461.1 [M+Na]+.

Aufarbeitung

  1. temperatureThe resulting mixture was heated at 50° C. under a reflux condenser under nitrogen for 71 h
  2. customDichloromethane was removed under reduced pressure
  3. additionThe residue was diluted with ethyl acetate
  4. washwashed with water
  5. extractionThe water layer was extracted with ethyl acetate
  6. washThe combined organics were washed with brine
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure
  10. customThe residue was triturated with 30% ethyl acetate in hexane and solids
  11. filtrationcollected by vacuum filtration
  12. concentrationThe filtrate was concentrated under reduced pressure
  13. custompurified
  14. additionFractions containing the desired product
  15. customobtained by filtration
  16. concentrationconcentrated under reduced pressure
  17. customThe residue was dried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-655f8d4e247847569d52efc58ef31201
Quelldatensatz
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09193692B2

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