反応 #657347
ord-130b3c9341e44780a9503cc14b7efe92
反応方程式
CHCl3
Methyl N-{[(9H-fluoren-9-ylmethyl)oxy]carbonyl}-L-α-aspartyl chloride
[2-amino-5-(methyloxy)phenyl](4-chlorophenyl)methanone
→
Methyl N1-[2-[(4-chlorophenyl)carbonyl]-4-(methyloxy)phenyl]-N2-{[(9H-fluoren-9-ylmethyl)oxy]carbonyl}-L-α-asparaginate
反応物
試薬
なし
反応条件
温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度before being cooled
- 2濃縮concentrated under reduced pressure
- 3その他used without further purification
実験手順
A mixture of Methyl N-{[(9H-fluoren-9-ylmethyl)oxy]carbonyl}-L-α-aspartyl chloride (prepared from J. Org. Chem. 1990, 55, 3068-3074 and J. Chem. Soc. Perkin Trans. 1 2001, 1673-1695) (221 g, 0.57 mol) and [2-amino-5-(methyloxy)phenyl](4-chlorophenyl)methanone (for a preparation see Intermediate 7) (133 g, 0.5 mol) in CHCl3 (410 mL) was stirred at 60° C. for 1.5 h before being cooled and concentrated under reduced pressure and used without further purification. LC/MS: m/z 613 [M(35Cl)+H]+, Rt=3.89 min.