Dichloromethane → Imidazole-1-carboxylic acid (8-tert-butyl-4,5-dihydro-thiazolo[4,5-h]quinazolin-2-yl)-amide
Reaktionsgleichung
[C:1]([C:5]1[N:14]=[CH:13][C:12]2[CH2:11][CH2:10][C:9]3[N:15]=[C:16]([NH2:18])[S:17][C:8]=3[C:7]=2[N:6]=1)([CH3:4])([CH3:3])[CH3:2].[CH:19]1[N:23]=[CH:22][N:21]([C:24](N2C=NC=C2)=[O:25])[CH:20]=1.C(Cl)Cl>CN(C=O)C>[C:1]([C:5]1[N:14]=[CH:13][C:12]2[CH2:11][CH2:10][C:9]3[N:15]=[C:16]([NH:18][C:24]([N:21]4[CH:20]=[CH:19][N:23]=[CH:22]4)=[O:25])[S:17][C:8]=3[C:7]=2[N:6]=1)([CH3:4])([CH3:2])[CH3:3]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 4 °C
Versuchsvorschrift
8-tert-Butyl-4,5-dihydro-thiazolo[4,5-h]quinazolin-2-ylamine (Stage A.1, 0.319 g, 1.225 mmol) and CDI (278 mg, 1.715 mmol) were added to DCM (5 ml) and DMF (0.25 ml) under an argon atm. After 18 h the residue was cooled to 4° C. and the precipitate was collected by filtration. The solid was dried at 50° C. in high vacuo to give the title compound as a pale yellow solid. LCMS: tR 0.95 min and M+H 319.0 (method A2) for (8-tert-butyl-4,5-dihydro-thiazolo[4,5-h]quinazolin-2-yl)-carbamic acid methyl ester; the product of the reaction of the title compound with MeOH during the preparation of the sample as MeOH solution.
Aufarbeitung
- filtrationthe precipitate was collected by filtration
- customThe solid was dried at 50° C. in high vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-f0060a546aca4b29adc7e2fed8c88a86
- Quelldatensatz
- uspto-grants-2013_01
- Patentnummer
- US08357707B2
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