Trifluoroacetic acid → HCID 23136941, Verbindung

HRID 242675Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 242675
C(OC([N:8]1[CH2:12][CH2:11][CH:10]([N:13]([CH2:22][C:23](=[O:25])[NH2:24])[CH2:14][C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=2)[CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[Cl:21][C:18]1[CH:19]=[CH:20][C:15]([CH2:14][N:13]([CH:10]2[CH2:11][CH2:12][NH:8][CH2:9]2)[CH2:22][C:23]([NH2:24])=[O:25])=[CH:16][CH:17]=1

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 66758387HCID 66758387, Verbindung

Produkt 1

HCID 23136941HCID 23136941, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution of 3-[carbamoylmethyl-(4-chloro-benzyl)-amino]-pyrrolidine-1-carboxylic acid tert-butyl ester (0.49 g, 1.32 mmol) in dichloromethane cooled at 0° C. was treated with trifluoroacetic acid (20%). The resulting mixture was warmed to room temperature and stirred for 2 h. The reaction mixture was concentrated in vacuo, diluted with ethyl acetate and free based with 10% aqueous sodium bicarbonate. The combined organics were dried over sodium sulfate. The product was used without any further purification ESI-MS m/z: 267 (M+1), UV retention time: 0.82 min.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additiondiluted with ethyl acetate
  3. dry with materialThe combined organics were dried over sodium sulfate
  4. customThe product was used without any further purification ESI-MS m/z

Quellen und Nachweise

ORD-Eintrag
ord-bdadf405822d42f8967d4cbce6434bfd
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08653096B2

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