1,2-Dichloroethane → (9H-Fluoren-9-yl)methyl(S)-1-((S)-1-((S)-1-((S)-1-amino-3-(4-hydroxyphenyl)-1-oxopropan-2-ylamino)-1-oxopropan-2-ylamino)-1-oxopropan-2-ylamino)-3-(4-hydroxyphenyl)-1-oxopropan-2-ylcarbamate

関与物質

反応手順

Following the procedure described in Example 7, except using (S)-2-amino-N-((S)-1-((S)-1-amino-3-(4-hydroxyphenyl)-1-oxopropan-2-ylamino)-1-oxopropan-2-yl)propanamide (40 mg, 0.124 mmol), Fmoc-L Tyrosine (52.6 mg, 0.130 mmol), 1-hydroxy-7-azabenzotriazole (9.5 mg, 0.070 mmol), anhydrous DMF (1.2 mL), N-methylmorpholine (16 μL, 0.146 mmol), EDC (28.5 mg, 0.149 mmol) and stirring at room temp for 4 h 15 min, 48.4 mg (47.5%) of the title compound is isolated as an off white solid. Purification is done by preparative HPLC (Condition A) using a PHENOMENEX® Luna Axia 30×100 mm S10 column from 35% Solvent B to 100% Solvent B over 11 min, ret. T=8.79 min. LC/MS (Condition A): ret. T=3.46 min, (M+H)+ 708.32. Analytical HPLC: (Condition A): >99%, ret. T=21.87 min, (Condition B): >99%, ret. T=22.15 min, (Condition C): >98%, ret. T=13.82 min, (Condition D): >99%, ret. T=12.79 min.

情報源と証拠