Triethylamine chloroform → Benzoyl chloride
Reaktionsgleichung
C(N(CC)CC)C.C(Cl)(Cl)[Cl:9].C[O:13][C:14](=O)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1NC(=O)CC1C=CC(OC2C=CC(O[C@H]3CC[C@@H](N)CC3)=CC=2)=CC=1>>[C:14]([Cl:9])(=[O:13])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1Komponenten
3
Versuchsvorschrift
A reactor was charged with 358 μl (1.7 eq, 179 μmol) of 0.5M triethylamine-chloroform solution containing 420 μl (105 μmol, 50 mg) of 2-(2-(4-(4-(cis-4-aminocyclohexyloxy)phenoxy)phenyl)acetylamino)benzoic acid methyl ester (0.25M-CHCl3) obtained by the Example 17, benzoyl chloride (1.5 eq, 22 mg) was added thereto and the mixture was stirred for 2.5 hours. After completing the reaction, 139 mg (157.5 μmol) of an aminomethylated polystyrene resin (product of Novabiochem) was added to the system and stirred for 12 hours. The solution was put on a Silica cartridge (product of Waters) and developed with a hexane/ethyl acetate mixture (1/2) and the obtained solution was distilled to remove the solvent.
Quellen und Nachweise
- ORD-Eintrag
- ord-460ffced0da741588ce93ed19f2ada17
- Quelldatensatz
- uspto-grants-2005_05
- Patentnummer
- US06890932B2
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