Reaktion #156710

Reaktionsgleichung

solution

(2S,4R)-4-(2-Chloro-4-methoxy-benzenesulfonyl)-1-[3-(5-chloro-pyridin-2-yl)-azetidine-3-carbonyl]-pyrrolidine-2-carboxylic acid (1-cyano-cyclopropyl)-amide

methyl iodide

methyl iodide

→

(2S,4R)-4-(2-Chloro-4-methoxy-benzenesulfonyl)-1-[3-(5-chloro-pyridin-2-yl)-1-methyl-azetidine-3-carbonyl]-pyrrolidine-2-carboxylic acid (1-cyano-cyclopropyl)-amide

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAfter complete addition the mixture
2. 2
   workup.STIRRINGthe mixture was stirred at 80° C. for 2 h
3. 3
   workup.WAITat 20° C. over night
4. 4
   SonstigeThe mixture was purified by preparative HPLC
5. 5
   Sonstigeto yield a colorless solid (3 mg; 6%)

Vorschrift

To a solution of example 2 (0.05 g, 86.4 μmol, Eq: 1.00) in refluxing methanol (1 ml) was added methyl iodide (9.2 mg, 4.05 μl, 64.8 μmol, Eq: 0.75). After complete addition the mixture was stirred at 80° C. for 2 h. Additional methyl iodide (9.2 mg, 4.05 μl, 64.8 μmol, Eq: 0.75) was added and the mixture was stirred at 80° C. for 2 h, then at 20° C. over night. The mixture was purified by preparative HPLC to yield a colorless solid (3 mg; 6%). m/z=592.2 [M+H]+.

Quelle