Potassium Carbonate → 6'-Ethynyl-2-fluoro-5-(4-piperidin-1-ylmethylphenyl)-[3,4']bipyridinyl-3'-ylamine

HRID 1506068Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1506068
C[Si]([C:5]#[C:6][C:7]1[N:12]=[CH:11][C:10]([NH2:13])=[C:9]([C:14]2[C:15]([F:33])=[N:16][CH:17]=[C:18]([C:20]3[CH:25]=[CH:24][C:23]([CH2:26][N:27]4[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]4)=[CH:22][CH:21]=3)[CH:19]=2)[CH:8]=1)(C)C.C(=O)([O-])[O-].[K+].[K+]>CO.C(Cl)Cl>[C:6]([C:7]1[N:12]=[CH:11][C:10]([NH2:13])=[C:9]([C:14]2[C:15]([F:33])=[N:16][CH:17]=[C:18]([C:20]3[CH:21]=[CH:22][C:23]([CH2:26][N:27]4[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]4)=[CH:24][CH:25]=3)[CH:19]=2)[CH:8]=1)#[CH:5]

Komponenten

5

Edukt 2

HCID 11430Potassium CarbonateHCID 582665496'-((Trimethylsilyl)ethynyl)-2-fluoro-5-(4-piperidin-1-ylmethyl-phenyl)-[3,4']bipyridinyl-3'-ylamine

Produkt 1

HCID 582664586'-Ethynyl-2-fluoro-5-(4-piperidin-1-ylmethylphenyl)-[3,4']bipyridinyl-3'-ylamine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittel2×HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 6′-((trimethylsilyl)ethynyl)-2-fluoro-5-(4-piperidin-1-ylmethyl-phenyl)-[3,4′]bipyridinyl-3′-ylamine (90 mg, 0.2 mmol) and potassium carbonate (150 mg, 1.1 mmol) in methanol (2 mL) was stirred at ambient temperature for 1 h. The cooled reaction mixture was diluted with DCM (20 mL) and methanol (2 mL) and washed with water (15 mL). The organic phase was separated, dried over sodium sulfate, filtered and evaporated in vacuo to afford a brown residue that was taken to the next step without purification.

Aufarbeitung

  1. customThe cooled reaction mixture
  2. washwashed with water (15 mL)
  3. customThe organic phase was separated
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. customto afford a brown residue that
  8. customwas taken to the next step without purification

Quellen und Nachweise

ORD-Eintrag
ord-9a6a25001fd94d639edda420d73c8d1f
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09216980B2

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