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Hexane → HCID 59852752, Verbindung

HRID 2373932
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2373932
[CH2:1]([O:8][C:9]1[C:10]([F:24])=[C:11]([CH:15]([C:17]2[C:22](Cl)=[N:21][CH:20]=[CH:19][N:18]=2)O)[CH:12]=[CH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Li]CCCC.CCCCCC.C[C:37]1(C)[CH2:42][CH2:41][CH2:40][C:39](C)(C)[NH:38]1.ClC1C=NC=C[N:48]=1.C(OC1C(F)=C(C=CC=1)C=O)C1C=CC=CC=1>C1COCC1>[NH2:48][C:22]1[C:17]2[N:18]([C:39]([CH:40]3[CH2:41][CH2:42][CH2:37]3)=[N:38][C:15]=2[C:11]2[CH:12]=[CH:13][CH:14]=[C:9]([O:8][CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[C:10]=2[F:24])[CH:19]=[CH:20][N:21]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 6

HCID 8058HexaneHCID 130352,2,6,6-TetramethylpiperidineHCID 73277ChloropyrazineHCID 561331Benzaldehyde, 2-fluoro-3-(phenylmethoxy)-HCID 59852791HCID 59852791, VerbindungHCID 178418339Butyllithium

Produkt 1

HCID 59852752
HCID 59852752, Verbindung
Ausbeute 21 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
-40 °C

Versuchsvorschrift

(3-Benzyloxy-2-fluorophenyl) (3-chloropyrazin-2-yl) carbinol: In a 100 mL three-necked round-bottom flask equipped with a N2-inlet and a thermometer was placed THF (28 mL). This was cooled to −40° C. and there was added 2.5 M solution of n-BuLi in hexane (11.52 mL, 28.8 mmole) followed by 2,2,6,6-tetramethylpiperidine (4.84 mL, 28.8 mmole). The temperature of the mixture was allowed to rise to 0° C. and stirring was continued at −5 to 0° C. for 30 minutes. The mixture was then cooled to −70° C., and the chloropyrazine (1.28 mL, 14.4 mmole) was added slowly over 15 minutes and the stirring was continued for 30 minutes. A solution of 3-benzyloxy-2-fluorobenzaldehyde (3.04 g. 13.2 mmole) in THF (7 mL) was then added at −70° C. and stirring was continued at −70 to −60° C. for 2 h. There after the temperature was allowed to rise to room temperature over 1 h. The reaction mixture was quenched with 2 N HCl (6 mL) and stirred overnight at room temperature. The mixture was then evaporated on a rotary evaporator to remove most of the THF. Ethyl acetate (20 mL) was added to the residue. The organic layer was separated, washed with water (10 mL), finally with brine (10 mL), dried over Na2SO4, filtered and concentrated. The crude residue obtained was 4.4 g. The above reaction was repeated four times and the products were combined. This was purified by silica-gel column chromatography using as the eluent ethyl acetate:hexane (30:70) and the title compound (3.8 g, 21%) was obtained.

Aufarbeitung

  1. customto rise to 0° C.
  2. temperatureThe mixture was then cooled to −70° C.
  3. waitthe stirring was continued for 30 minutes
  4. stirringstirring
  5. waitwas continued at −70 to −60° C. for 2 h
  6. waitto rise to room temperature over 1 h
  7. customThe reaction mixture was quenched with 2 N HCl (6 mL)
  8. stirringstirred overnight at room temperature
  9. customThe mixture was then evaporated on a rotary evaporator
  10. customto remove most of the THF
  11. additionEthyl acetate (20 mL) was added to the residue
  12. customThe organic layer was separated
  13. washwashed with water (10 mL), finally with brine (10 mL)
  14. dry with materialdried over Na2SO4
  15. filtrationfiltered
  16. concentrationconcentrated
  17. customThe crude residue obtained
  18. customThe above reaction
  19. customThis was purified by silica-gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-bd666c95d1e84a26becaa6a3fd80fbe6
Quelldatensatz
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07459554B2

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