Dichloromethane → HCID 67235119, Verbindung

HRID 1505318Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1505318
[CH3:1][C@@H:2]([NH:22]C(=O)OC(C)(C)C)[C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[C:15]([O:20][CH3:21])[CH:14]=2)=[CH:8][CH:7]=1)=[O:4].ClCCl>>[CH3:19][C:16]1[CH:17]=[CH:18][C:13]([O:12][C:9]2[CH:10]=[CH:11][C:6]([NH:5][C:3](=[O:4])[C@@H:2]([CH3:1])[NH2:22])=[CH:7][CH:8]=2)=[CH:14][C:15]=1[O:20][CH3:21]

Komponenten

3

Edukt 2

HCID 6344DichloromethaneHCID 68322429HCID 68322429, Verbindung2×

Produkt 1

HCID 67235119HCID 67235119, VerbindungAusbeute 97,3 %

Versuchsvorschrift

To a solution of 1,1-dimethylethyl {(1R)-1-methyl-2-[(4-{[4-methyl-3-(methyloxy)phenyl]oxy}phenyl)amino]-2-oxoethyl}carbamate (Intermediate 21, 300 mg) in dry dichloromethane (7.5 mL) TFA (2.5 mL, 32.4 mmol) was slowly added and the reaction mixture was stirred for 1.5 hours at room temperature. The solvent and the excess of TFA were evaporated and the residue was purified by SCX cartridge (10 g) to afford the title compound as an orange oil (219 mg).

Aufarbeitung

  1. customThe solvent and the excess of TFA were evaporated
  2. customthe residue was purified by SCX cartridge (10 g)

Quellen und Nachweise

ORD-Eintrag
ord-5fc28f03edb34c5c944f156534275047
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09216967B2

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