Sodium Iodide → Acetic acid 3-[4-(2-tert-butyl-6-cyclopropyl-pyrimidin-4-yl)-piperazin-1-yl]-propyl ester
Reaktionsgleichung
[C:1]([C:5]1[N:10]=[C:9]([N:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)[CH:8]=[C:7]([CH:17]2[CH2:19][CH2:18]2)[N:6]=1)([CH3:4])([CH3:3])[CH3:2].Cl[CH2:21][CH2:22][CH2:23][O:24][C:25](=[O:27])[CH3:26].C(N(CC)CC)C.[I-].[Na+]>CN(C)C=O>[C:1]([C:5]1[N:10]=[C:9]([N:11]2[CH2:12][CH2:13][N:14]([CH2:21][CH2:22][CH2:23][O:24][C:25](=[O:27])[CH3:26])[CH2:15][CH2:16]2)[CH:8]=[C:7]([CH:17]2[CH2:19][CH2:18]2)[N:6]=1)([CH3:4])([CH3:2])[CH3:3]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 80 °C
Versuchsvorschrift
2.9 g of 2-tert-Butyl-4-piperazin-1-yl-6-cyclopropyl-pyrimidine (11.1 mmol), 1.8 g acetic acid 3-chloro-propyl ester (13.2 mmol), 1.38 g of triethylamine (13.7 mmol), and a spatula tip of sodium iodide were dissolved in 50 ml of dimethylformamide and stirred for 8 h at 80° C. After cooling to room temperature, the dimethylformamide was evaporated. The reaction mixture was partitioned between water and ethyl acetate. The organic layer was dried over magnesium sulfate, filtered, and the solvent was evaporated. The crude product (3.7 g) was directly used in the subsequent reaction step.
Aufarbeitung
- temperatureAfter cooling to room temperature
- customthe dimethylformamide was evaporated
- customThe reaction mixture was partitioned between water and ethyl acetate
- dry with materialThe organic layer was dried over magnesium sulfate
- filtrationfiltered
- customthe solvent was evaporated
- customThe crude product (3.7 g) was directly used in the subsequent reaction step
Quellen und Nachweise
- ORD-Eintrag
- ord-184b0733e8444260864a6e980e6ad5c3
- Quelldatensatz
- uspto-grants-2012_06
- Patentnummer
- US08202868B2
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