Triethylsilane → HCID 66635174, Verbindung

HRID 510144Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 510144
COC1C=C(OC)C=CC=1C[N:6]1[C:10]2[N:11]=[C:12]([C:15]3[C:23]4[C:18](=[N:19][CH:20]=[C:21]([F:24])[CH:22]=4)[N:17]([CH2:25][C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=4[F:32])[N:16]=3)[N:13]=[CH:14][C:9]=2[N:8]([CH3:33])[S:7]1(=[O:35])=[O:34].C([SiH](CC)CC)C>FC(F)(F)C(O)=O>[F:24][C:21]1[CH:22]=[C:23]2[C:15]([C:12]3[N:13]=[CH:14][C:9]4[N:8]([CH3:33])[S:7](=[O:34])(=[O:35])[NH:6][C:10]=4[N:11]=3)=[N:16][N:17]([CH2:25][C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=3[F:32])[C:18]2=[N:19][CH:20]=1

Komponenten

4

Edukt 2

HCID 12052TriethylsilaneHCID 66634917HCID 66634917, Verbindung

Produkt 1

HCID 66635174HCID 66635174, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Versuchsvorschrift

28 mg (0.050 mmol) of the compound from example 100A were dissolved in 1.5 ml of trifluoroacetic acid and then admixed with 79 μl (0.495 mmol) of triethylsilane, and the mixture was heated to reflux overnight. This was followed by concentration to dryness. After purification by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient), this gave 10.4 mg (48% of theory) of the title compound.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureto reflux overnight
  3. concentrationThis was followed by concentration to dryness
  4. customAfter purification by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient)

Quellen und Nachweise

ORD-Eintrag
ord-11dc3467c9e14bc6bb633252a589f161
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09096592B2

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