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Hydrochloric Acid → HCID 67009332, Verbindung

HRID 1630043
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1630043
[CH2:1]([O:8][CH2:9][CH:10]([NH:14]C(OC(C)(C)C)=O)[C:11]([OH:13])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.[O:55]([C:62]1[CH:68]=[CH:67][C:65]([NH2:66])=[CH:64][CH:63]=1)[C:56]1[CH:61]=[CH:60][CH:59]=[CH:58][CH:57]=1.Cl>O1CCOCC1.CN(C=O)C>[NH2:14][CH:10]([CH2:9][O:8][CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[C:11]([NH:66][C:65]1[CH:64]=[CH:63][C:62]([O:55][C:56]2[CH:61]=[CH:60][CH:59]=[CH:58][CH:57]=2)=[CH:68][CH:67]=1)=[O:13]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 313Hydrochloric AcidHCID 8764(4-Aminophenoxy)benzeneHCID 81531DiisopropylethylamineHCID 3334623-(Benzyloxy)-2-((tert-butoxycarbonyl)amino)propanoic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

Produkt 1

HCID 67009332
HCID 67009332, Verbindung
Ausbeute 33 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A flask was charged with 3-benzyloxy-2-tert-butoxycarbonylaminopropionic acid (5.0 g, 16.9 mmoles), HATU (7.0 g, 18.6 mmoles) and DMF (5 mL). DIEA (8.8 mL, 50.7 mmoles) was added and the mixture was stirred for 15 minutes. 4-Phenoxyaniline (3.4 g, 18.6 mmoles) was added and the mixture was stirred at ambient temperature for 18 hours. The reaction mixture was partitioned between ethyl acetate and deionized water. The aqueous layer was separated and extracted twice with ethyl acetate. The combined extract was washed sequentially with 5% lithium chloride (3×10 mL), 1N sodium bicarbonate (2×10 mL), 5% citric acid (2×10 mL), deionized water (2×10 mL) and then brine (1×10 mL), dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The crude material was recrystallized from methanol to afford a white solid. The solid was combined with 4N hydrogen chloride in dioxane (25 mL). The mixture was stirred at ambient temperature for 18 hours. Volatiles then were removed under rotary evaporation. The resultant oil was partitioned between 1N sodium bicarbonate and ethyl acetate. The aqueous layer was extracted with ethyl acetate. The combined extract was washed with brine (2×10 mL), dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The crude was recrystallized from methanol to give 2-amino-3-benzyloxy-N-(4-phenoxyphenyl)propanamide (2 g, 5.47 mmoles, 33% yield), as an off-white solid. 1H-NMR (400 MHz, CDCl3): δ 9.55 (s, 1H), 7.60-7.50 (m, 2H), 7.40-7.27 (m, 5H), 7.08 (t, 1H), 7.01-6.95 (m, 3H), 4.57 (t, 2H), 3.85-3.70 (m, 3H), 1.97 (2, 2H). MS (D) for C22H22N2O3. found 363.0 (MH+).

Aufarbeitung

  1. stirringthe mixture was stirred at ambient temperature for 18 hours
  2. customThe reaction mixture was partitioned between ethyl acetate
  3. customThe aqueous layer was separated
  4. extractionextracted twice with ethyl acetate
  5. extractionThe combined extract
  6. washwas washed sequentially with 5% lithium chloride (3×10 mL), 1N sodium bicarbonate (2×10 mL), 5% citric acid (2×10 mL), deionized water (2×10 mL)
  7. dry with materialbrine (1×10 mL), dried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe crude material was recrystallized from methanol
  11. customto afford a white solid
  12. stirringThe mixture was stirred at ambient temperature for 18 hours
  13. customVolatiles then were removed under rotary evaporation
  14. customThe resultant oil was partitioned between 1N sodium bicarbonate and ethyl acetate
  15. extractionThe aqueous layer was extracted with ethyl acetate
  16. extractionThe combined extract
  17. washwas washed with brine (2×10 mL)
  18. dry with materialdried over anhydrous sodium sulfate
  19. filtrationfiltered
  20. concentrationconcentrated in vacuo
  21. customThe crude was recrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-91a2803a37ca40c6b2d140cdcc66bcb7
Quelldatensatz
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08791102B2

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