Reaktionsgleichung
[C:1]([O:5][C:6](=[O:13])[C:7]([CH3:12])([CH3:11])[C:8]([OH:10])=[O:9])([CH3:4])([CH3:3])[CH3:2].ClCCl.[CH:17]1(O)[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1.CCN=C=NCCCN(C)C>CN(C1C=CN=CC=1)C.CC(OC)(C)C>[CH:17]1([O:9][C:8](=[O:10])[C:7]([CH3:12])([CH3:11])[C:6]([O:5][C:1]([CH3:4])([CH3:2])[CH3:3])=[O:13])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1Komponenten
7
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
To a mixture of 2,2-dimethylmalonic acid mono-t-butyl ester [CAS No. 143688-40-8] (800 mg), DMAP (104 mg), and dichloromethane (8 mL), cyclohexanol (0.494 mL) and WSC (976 mg) were sequentially added at 0° C. The resulting mixture was stirred overnight at room temperature, and TBME (50 mL) was added thereto. The resulting mixture was sequentially washed with water (30 mL) and saturated aqueous sodium chloride solution (30 mL), and dried over anhydrous magnesium sulfate. The resulting mixture was filtered, and the filtrate obtained was concentrated under reduced pressure. The residue obtained was purified by silica gel column chromatography (mixed solvent of heptane-ethyl acetate) to obtain the captioned compound (817 mg).
Aufarbeitung
- washThe resulting mixture was sequentially washed with water (30 mL) and saturated aqueous sodium chloride solution (30 mL)
- dry with materialdried over anhydrous magnesium sulfate
- filtrationThe resulting mixture was filtered
- customthe filtrate obtained
- concentrationwas concentrated under reduced pressure
- customThe residue obtained
- customwas purified by silica gel column chromatography (mixed solvent of heptane-ethyl acetate)
Quellen und Nachweise
- ORD-Eintrag
- ord-fa9d8e23bd104a26acf716c18aadbbc6
- Quelldatensatz
- uspto-grants-2013_05
- Patentnummer
- US08436009B2
Verknüpfte Notizen
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