反应详情

Boc-L-Glu(OBzl)OSu (Bachem, 434 mg (1 mmol) is reacted with L-Ala-OtBu.HCl, 182 mg (1 mmol) in 10 mL DMF containing triethylamine (202 mg). After stirring for 16 hours at room temperature, the reaction mixture is rotary evaporated to dryness and the residue is redissolved in methylene chloride, washed with water, dried over sodium sulfate and evaporated to dryness. The residue is redissolved in methanol, 50 mL, and transferred to a Parr flask. 10% Pd/C catalyst (Aldrich), 50 mg, is added and the flask is charged with 40 psi hydrogen gas on a Parr shaker. The mixture is shaken for 2 hours at room temperature or until no further consumption of hydrogen is noted. The Parr flask is evacuated and charged with argon gas. The mixture is filtered through Celite, and the filtrate is rotary evaporated to give crude Boc-L-Glu-Ala-OtBu.

1. customthe reaction mixture is rotary evaporated to dryness
2. dissolutionthe residue is redissolved in methylene chloride
3. washwashed with water
4. dry with materialdried over sodium sulfate
5. customevaporated to dryness
6. dissolutionThe residue is redissolved in methanol
7. addition10% Pd/C catalyst (Aldrich), 50 mg, is added
8. additionthe flask is charged with 40 psi hydrogen gas on a Parr shaker
9. stirringThe mixture is shaken for 2 hours at room temperature or until no further consumption of hydrogen
10. customThe Parr flask is evacuated
11. additioncharged with argon gas
12. filtrationThe mixture is filtered through Celite
13. customthe filtrate is rotary evaporated