Potassium Carbonate → 2-(Benzotriazol-1-yl)methyl-8-(4,6-dimethoxy-pyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4,5]decane
Reaktionsgleichung
[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[N:2]1.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:17][CH:18]1[CH2:22][O:21][C:20]2([CH2:27][CH2:26][N:25]([C:28]3[N:33]=[C:32]([O:34][CH3:35])[CH:31]=[C:30]([O:36][CH3:37])[N:29]=3)[CH2:24][CH2:23]2)[O:19]1>CN(C)C=O>[N:1]1([CH2:17][CH:18]2[CH2:22][O:21][C:20]3([CH2:23][CH2:24][N:25]([C:28]4[N:29]=[C:30]([O:36][CH3:37])[CH:31]=[C:32]([O:34][CH3:35])[N:33]=4)[CH2:26][CH2:27]3)[O:19]2)[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[N:2]1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 120 °C
Versuchsvorschrift
To 37.63 gm (0.3163 mole) of benzotriazole and 35 gm of potassium carbonate in Dimethylformamide (DMF) (350 ml) was added slowly under stirring 82 gm of 2-chloromethyl-8-(4,6-dimethoxy-pyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4,5]decane (intermediate for compound 7) in DMF (300 ml). After the addition, reaction mixture was heated to 120° C. and maintained for 30 hrs. The reaction mixture was cooled to room temperature 28° C. and filtered. The solvent was distilled off to get the product. It was a thick dark brown liquid. Yield of product was 90%
Aufarbeitung
- additionAfter the addition, reaction mixture
- temperaturemaintained for 30 hrs
- temperatureThe reaction mixture was cooled to room temperature 28° C.
- filtrationfiltered
- distillationThe solvent was distilled off
- customto get the product
Quellen und Nachweise
- ORD-Eintrag
- ord-e1d09784d5e745e89ef2dfc6d17429fa
- Quelldatensatz
- uspto-grants-2014_09
- Patentnummer
- US08841296B2
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