Trifluoroacetic acid → HCID 89720591, Verbindung

HRID 623992Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 623992
[CH:1]1([CH2:4][O:5][C:6]23[CH2:15][CH:10]4[CH2:11][CH:12]([CH2:14][CH:8]([N:9]4C(OC(C)(C)C)=O)[CH2:7]2)[CH2:13]3)[CH2:3][CH2:2]1.FC(F)(F)C(O)=O>C(Cl)Cl>[CH:1]1([CH2:4][O:5][C:6]23[CH2:15][CH:10]4[CH2:11][CH:12]([CH2:14][CH:8]([NH:9]4)[CH2:7]2)[CH2:13]3)[CH2:3][CH2:2]1

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 89720588HCID 89720588, Verbindung

Produkt 1

HCID 89720591HCID 89720591, VerbindungAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a 50 mL RB flask fitted with magnetic stirrer was charged tert-butyl 5-(cyclopropylmethoxy)-2-azatricyclo[3.3.1.13,7]decane-2-carboxylate, Intermediate-19 (50 mg, 0.016 mmol) in DCM (5 mL). Then reaction mixture was cooled to 0° C. and trifluoroacetic acid (0.099 g, 0.084 mmol) was added and stirred for 4 hours. After completion of the reaction (reaction was monitored by LCMS) the reaction mixture was concentrated followed by trituration with mixture of hexane:ether (1:1) to give Intermediate-20 (50 mg, yield=95%) as an oily mass.

Aufarbeitung

  1. customTo a 50 mL RB flask fitted with magnetic stirrer
  2. customThen reaction mixture
  3. customAfter completion of the reaction (reaction was monitored by LCMS) the reaction mixture
  4. concentrationwas concentrated
  5. additionfollowed by trituration with mixture of hexane:ether (1:1)
  6. customto give Intermediate-20 (50 mg, yield=95%) as an oily mass

Quellen und Nachweise

ORD-Eintrag
ord-53c872ebcd3040579693ab3ba35c90cd
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09303016B2

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