Trifluoroacetic acid → (5-Methylthiophen-2-yl)(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)methanone trifluoroacetate

HRID 1689209

Reaktionsgleichung

Reaktionsgleichung von HRID 1689209
[CH3:1][C:2]1[S:6][C:5]([C:7]([N:9]2[CH2:14][C:13]3([CH2:19][CH2:18][N:17](C(OC(C)(C)C)=O)[CH2:16][CH2:15]3)[O:12][CH2:11][CH2:10]2)=[O:8])=[CH:4][CH:3]=1.[F:27][C:28]([F:33])([F:32])[C:29]([OH:31])=[O:30]>C(Cl)Cl>[F:27][C:28]([F:33])([F:32])[C:29]([OH:31])=[O:30].[CH3:1][C:2]1[S:6][C:5]([C:7]([N:9]2[CH2:14][C:13]3([CH2:19][CH2:18][NH:17][CH2:16][CH2:15]3)[O:12][CH2:11][CH2:10]2)=[O:8])=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 57989101Tert-butyl 4-(5-methylthiophene-2-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecane-9-carboxylate

Produkt 1

HCID 67292300(5-Methylthiophen-2-yl)(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)methanone trifluoroacetate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

tert-Butyl 4-(5-methylthiophene-2-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecane-9-carboxylate u) (example 9, step a) (0.32 g) in DCM (3 mL) was treated with trifluoroacetic acid (1.0 g). After 2 h, the reaction mixture was evaporated in vacuo and azeotroped twice with toluene to yield the subtitled compound which was used directly. Yield 0.32 g.

Aufarbeitung

  1. customthe reaction mixture was evaporated in vacuo
  2. customazeotroped twice with toluene

Quellen und Nachweise

ORD-Eintrag
ord-775c23e9d857488ebd5c4276ea78e8d1
Quelldatensatz
uspto-grants-2012_04
Patentnummer
US08148373B2

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