StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Ammonium Chloride → HCID 21070520, Verbindung

HRID 1371731
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1371731
Br[C:2]1[C:3]([Cl:9])=[N:4][C:5]([Cl:8])=[N:6][CH:7]=1.C([Mg]Cl)(C)C.[C:15]([Si:19]([CH3:34])([CH3:33])[O:20][C:21]1[C:22]([O:31][CH3:32])=[C:23]([C:26]([F:30])=[C:27]([F:29])[CH:28]=1)[CH:24]=[O:25])([CH3:18])([CH3:17])[CH3:16].[Cl-].[NH4+]>O1CCCC1.O.C(OCC)(=O)C>[C:15]([Si:19]([CH3:34])([CH3:33])[O:20][C:21]1[C:22]([O:31][CH3:32])=[C:23]([CH:24]([C:2]2[C:3]([Cl:9])=[N:4][C:5]([Cl:8])=[N:6][CH:7]=2)[OH:25])[C:26]([F:30])=[C:27]([F:29])[CH:28]=1)([CH3:18])([CH3:17])[CH3:16]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 25517Ammonium ChlorideHCID 2899735-Bromo-2,4-dichloropyrimidineHCID 21070519HCID 21070519, VerbindungHCID 178418918HCID 178418918, Verbindung

Produkt 1

HCID 21070520HCID 21070520, VerbindungAusbeute 65 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962
Water
Lösungsmittel
HCID 8028TetrahydrofuranLösungsmittel2×
HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
-30 °C

Versuchsvorschrift

To a solution of 5-bromo-2,4-dichloropyrimidine (753.6 mg, 3.307 mmol, Matrix Chemicals) in tetrahydrofuran (20 mL) cooled to −30° C. was added dropwise isopropylmagnesium chloride. The temperature was maintained below −25° C. throughout the addition. At the end of addition, the reaction mixture was stirred at −30° C. for 20 minutes and a solution of 3-(tert-butyl-dimethyl-silanyloxy)-5,6-difluoro-2-methoxy-benzaldehyde (1 g, 3.307 mmol, Example 266) in tetrahydrofuran was added dropwise. The temperature was maintained below −25° C. throughout the addition. The reaction mixture was allowed to warm up to 0° C. after the addition was completed. After being stirred at 0° C. for 45 minutes, saturated solution of ammonium chloride (−3 mL) was added. The mixture was taken up in water and ethyl acetate. The aqueous layer was extracted with ethyl acetate. The combined organic layers were washed with brine and dried over anhydrous magnesium sulfate. The solids were filtered off and the filtrate was concentrated in vacuo. Purification of the crude residue by flash chromatography (Biotage system, 60 Å silica gel, eluting with 5–10% ethyl acetate in hexanes) yielded [3-(tert-butyl-dimethyl-silanyloxy)-5,6-difluoro-2-methoxy-phenyl]-(2,4-dichloro-pyrimidin-5-yl)-methanol as white solids (965 mg, 65%). LR-MS (M+) 451.1.

Aufarbeitung

  1. temperatureThe temperature was maintained below −25° C. throughout the addition
  2. additionAt the end of addition
  3. temperatureThe temperature was maintained below −25° C. throughout the addition
  4. temperatureto warm up to 0° C.
  5. additionafter the addition
  6. stirringAfter being stirred at 0° C. for 45 minutes
  7. extractionThe aqueous layer was extracted with ethyl acetate
  8. washThe combined organic layers were washed with brine
  9. dry with materialdried over anhydrous magnesium sulfate
  10. filtrationThe solids were filtered off
  11. concentrationthe filtrate was concentrated in vacuo
  12. customPurification of the crude residue
  13. washby flash chromatography (Biotage system, 60 Å silica gel, eluting with 5–10% ethyl acetate in hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-3f64164ab88e40a1828a7b7a9253cece
Quelldatensatz
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07157455B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion