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Hexane → (4S,6S)-4-(2-fluoro-5-(6-((trimethylsilyl)ethynyl)pyridin-3-yl)phenyl)-4-(fluoromethyl)-6-(trifluoromethyl)-5,6-dihydro-4H-1,3-oxazin-2-amine

HRID 930325
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 930325
P([O-])([O-])([O-])=O.[K+].[K+].[K+].[F:9][C:10]1[CH:15]=[CH:14][C:13](B2OC(C)(C)C(C)(C)O2)=[CH:12][C:11]=1[C@:25]1([CH2:36][F:37])[CH2:30][C@@H:29]([C:31]([F:34])([F:33])[F:32])[O:28][C:27]([NH2:35])=[N:26]1.Br[C:39]1[CH:40]=[CH:41][C:42]([C:45]#[C:46][Si:47]([CH3:50])([CH3:49])[CH3:48])=[N:43][CH:44]=1.CCCCCC>O1CCOCC1.O.O.C(C1C(C(C)(C)C)=C([Pd]Cl)C=CC=1NC)(C)(C)C>[F:9][C:10]1[CH:15]=[CH:14][C:13]([C:39]2[CH:44]=[N:43][C:42]([C:45]#[C:46][Si:47]([CH3:48])([CH3:50])[CH3:49])=[CH:41][CH:40]=2)=[CH:12][C:11]=1[C@:25]1([CH2:36][F:37])[CH2:30][C@@H:29]([C:31]([F:33])([F:32])[F:34])[O:28][C:27]([NH2:35])=[N:26]1
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Komponenten

8

Edukt 4

HCID 8058HexaneHCID 62657Potassium Phosphate, TribasicHCID 109995845-Bromo-2-[2-(trimethylsilyl)ethynyl]pyridineHCID 86732145(4S,6S)-4-(2-fluoro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)-4-(fluoromethyl)-6-(trifluoromethyl)-5,6-dihydro-4H-1,3-oxazin-2-amine

Produkt 1

HCID 86732153
(4S,6S)-4-(2-fluoro-5-(6-((trimethylsilyl)ethynyl)pyridin-3-yl)phenyl)-4-(fluoromethyl)-6-(trifluoromethyl)-5,6-dihydro-4H-1,3-oxazin-2-amine
Ausbeute 44,3 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 178482226HCID 178482226, VerbindungKatalysatorHCID 962WaterLösungsmittelHCID 218864351,4-Dioxane--water (1/1)Lösungsmittel

Versuchsvorschrift

A mixture of potassium phosphate (0.676 g, 3.19 mmol), (4S,6S)-4-(2-fluoro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)-4-(fluoromethyl)-6-(trifluoromethyl)-5,6-dihydro-4H-1,3-oxazin-2-amine (8b, 1.428 g, 3.40 mmol), 5-bromo-2-((trimethylsilyl)ethynyl)pyridine (0.270 g, 1.062 mmol) and 1,1-bis[(di-t-butyl-p-methylaminophenyl]palladium(II) chloride (0.038 g, 0.053 mmol) in dioxane/water (5.0/1.2 mL) was heated in microwave reactor at 110° C. for 35 min. The reaction mixture was diluted with water and extracted with DCM three times. The combined organic layers were washed with brine, dried on sodium sulfate, filtered and concentrated. The crude material was purified by silica gel chromatography: 0-100% EtOAc/hexane in 15 min. The product was obtained as an off-white solid. Trituration with hexane afforded the pure product as a white solid (0.22 g, 44% yield). MS m/z=468 [M+H]+. Calculated for C22H22F5N3OSi: 467.5.

Aufarbeitung

  1. extractionextracted with DCM three times
  2. washThe combined organic layers were washed with brine
  3. customdried on sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe crude material was purified by silica gel chromatography
  7. customThe product was obtained as an off-white solid

Quellen und Nachweise

ORD-Eintrag
ord-ded940f4a1494d38a1b5cccb9afe27b6
Quelldatensatz
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09296734B2

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