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Diethyl Ether → HCID 57758309, Verbindung

HRID 1094894
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1094894
[NH2:1][C:2]1[C:7]2=[C:8]([C:13]3[CH:18]=[CH:17][C:16]([NH:19][C:20]([NH:22][C:23]4[CH:28]=[C:27]([C:29]([F:32])([F:31])[F:30])[CH:26]=[CH:25][C:24]=4[F:33])=[O:21])=[CH:15][CH:14]=3)[C:9]([CH2:11]O)=[CH:10][N:6]2[N:5]=[CH:4][N:3]=1.S(Cl)(Cl)=O.CCC(C)[BH-](C(C)CC)C(C)CC.[Li+].CCOCC>C1COCC1.ClCCCl>[NH2:1][C:2]1[C:7]2=[C:8]([C:13]3[CH:14]=[CH:15][C:16]([NH:19][C:20]([NH:22][C:23]4[CH:28]=[C:27]([C:29]([F:30])([F:31])[F:32])[CH:26]=[CH:25][C:24]=4[F:33])=[O:21])=[CH:17][CH:18]=3)[C:9]([CH3:11])=[CH:10][N:6]2[N:5]=[CH:4][N:3]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 3283Diethyl EtherHCID 24386Thionyl ChlorideHCID 3611392Lithium tri-s-butylborohydrideHCID 57758061HCID 57758061, Verbindung

Produkt 1

HCID 57758309HCID 57758309, VerbindungAusbeute 84 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 11
1,2-Dichloroethane
Lösungsmittel
HCID 8028TetrahydrofuranLösungsmittel3×

Reaktionsbedingungen

Temperatur
-45 °C

Versuchsvorschrift

A suspension of N-{4-[4-amino-6-(hydroxymethyl)pyrrolo[2,1-f][1,2,4]-triazin-5-yl]phenyl}-N′-[2-fluoro-5-(trifluoromethyl)phenyl]urea (423 mg, 0.930 mmol) in THF 5 (mL) and 1,2-dichloroethane (5 mL) was treated with thionyl chloride (148 μL, 2.05 mmol) at rt. After 10 min the reaction appeared complete by RP-HPLC. After 30 min the reaction was concentrated under vacuum. The residue was suspended in 1,2-dichloroethane and sonicated briefly, then concentrated again under vacuum (2×). The resulting solid (412 mg, 0.86 mmol) was suspended in THF (20 mL) and cooled to −45° C. This suspension was treated with 1.0 M L-Selectride in THF (8.6 mL, 8.6 mmol). After 15 min the reaction was complete by HPLC. The reaction mixture was removed from the ice bath and quenched with MeOH (1 mL), then treated with 1 M sodium hydroxide (2 mL) and 30% hydrogen peroxide (2 mL). After 15 min stirring, the mixture was diluted with EtOAc (200 mL) and water (200 mL). The organic layer was washed with brine and dried with sodium sulfate. Concentration of the organic layer and trituration with ether:hexanes gave the title compound as an white powder (323 mg, 0.73 mmol, 84% yield). 1H-NMR (CD3OD-d6) δ 8.61 (d, J=8 Hz, 1H), 7.73 (s, 1H), 7.62 (d, J=9 Hz, 2H), 7.48 to 7.50 (m, 1H), 7.35 (d, J=9 Hz, 2H), 7.31 to 7.36 (m, 2H), 2.14 (s, 3H); MS [M+H]+=445.1; LCMS RT=2.80.

Aufarbeitung

  1. concentrationAfter 30 min the reaction was concentrated under vacuum
  2. customsonicated briefly
  3. concentrationconcentrated again under vacuum (2×)
  4. waitAfter 15 min the reaction was complete by HPLC
  5. customThe reaction mixture was removed from the ice bath
  6. customquenched with MeOH (1 mL)
  7. additiontreated with 1 M sodium hydroxide (2 mL) and 30% hydrogen peroxide (2 mL)
  8. additionthe mixture was diluted with EtOAc (200 mL) and water (200 mL)
  9. washThe organic layer was washed with brine
  10. dry with materialdried with sodium sulfate

Quellen und Nachweise

ORD-Eintrag
ord-3940f22da92344dfbce7cf1279900f14
Quelldatensatz
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08133995B2

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