Trifluoroacetic acid → HCID 178420112, Verbindung

HRID 1443380Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1443380
FC(F)(F)C(O)=O.C(OC([N:15]1[CH:24]([C:25]2[NH:26][CH:27]=[C:28]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)[N:29]=2)[CH2:23][C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:16]1)=O)(C)(C)C>>[C:30]1([C:28]2[N:29]=[C:25]([CH:24]3[CH2:23][C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[CH2:16][NH:15]3)[NH:26][CH:27]=2)[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1

Komponenten

3

Edukt 2

HCID 6422Trifluoroacetic acidHCID 178451477HCID 178451477, Verbindung

Produkt 1

HCID 178420112HCID 178420112, Verbindung

Versuchsvorschrift

Triflouroacetic acid (TFA) (4 mL) was cooled in a test tube to about 0° C. To the cool solvent was then added the product prepared in Step B (0.75 g, 2 mmol) above. The reaction mixture was allowed to warm to room temperature over about 45 minutes. Excess TFA was removed under a stream of N2 gas. The residue was partitioned between dichloromethane (15 mL) and saturated NaHCO3. The aqueous phase was then re-extracted with a second portion of dichloromethane and the organic phases combined, dried over MgSO4 and filtered, to yield the title compound in dichloromethane solution. The filtrate was used in the next step without further purification or isolation.

Aufarbeitung

  1. customExcess TFA was removed under a stream of N2 gas
  2. customThe residue was partitioned between dichloromethane (15 mL) and saturated NaHCO3
  3. extractionThe aqueous phase was then re-extracted with a second portion of dichloromethane
  4. dry with materialdried over MgSO4
  5. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-2961d1d5d5cb4ea79e22f188918c74ac
Quelldatensatz
uspto-grants-2010_02
Patentnummer
US07659402B2

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