Silane, ((1-methoxy-2-methyl-1-propenyl)oxy)trimethyl- → HCID 59251058, Verbindung

HRID 218127

Reaktionsgleichung

Reaktionsgleichung von HRID 218127
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:16]3[C:11](=[CH:12][C:13]([CH:17](O)[CH2:18][CH:19]([CH3:21])[CH3:20])=[CH:14][CH:15]=3)[CH:10]=[N:9]2)=[CH:4][CH:3]=1.[CH3:23][O:24][C:25]([O:29][Si](C)(C)C)=[C:26]([CH3:28])[CH3:27]>C(Cl)Cl.Cl[Ti](Cl)(Cl)Cl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:16]3[C:11](=[CH:12][C:13]([CH:17]([CH2:18][CH:19]([CH3:21])[CH3:20])[C:26]([CH3:28])([CH3:27])[C:25]([O:24][CH3:23])=[O:29])=[CH:14][CH:15]=3)[CH:10]=[N:9]2)=[CH:4][CH:3]=1

Komponenten

5

Edukt 2

HCID 552336Silane, ((1-methoxy-2-methyl-1-propenyl)oxy)trimethyl-HCID 67006196HCID 67006196, Verbindung

Produkt 1

HCID 59251058HCID 59251058, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 24193Titanium TetrachlorideKatalysatorHCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a solution of 1-(1-(4-fluorophenyl)-1H-indazol-5-yl)-3-methylbutan-1-ol (0.41 mmol) in 20 mL of CH2Cl2 at 0° C. was added 1M TiCl4 in CH2Cl2 (0.5 mmol) all at once. After 30 min, (1-methoxy-2-methylprop-1-enyloxy)trimethylsilane (0.24 mL, 1.2 mmol) was added and the reaction was warmed to rt and stirred overnight. The reaction was quenched with water and extracted with CH2Cl2. The CH2Cl2 extracts were dried over MgSO4, filtered, and concentrated by rotary evaporator to give methyl 3-(1-(4-fluorophenyl)-1H-indazol-5-yl)-2,2,5-trimethylhexanoate. MS found: (M+H)+=383.

Aufarbeitung

  1. customThe reaction was quenched with water
  2. extractionextracted with CH2Cl2
  3. dry with materialThe CH2Cl2 extracts were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated by rotary evaporator

Quellen und Nachweise

ORD-Eintrag
ord-e4fd128355604a5c878d80fa0409e38f
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08198311B2

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