反应详情

L-Alanine (3.57 g, 40 mmol) was dissolved in 18.8 ml of Triton B (40 mmol), evaporated to dryness, and the oily residue re-evaporated twice with DMF (30 ml each). The salt obtained was stirred with 11.45 g of Boc-Ala-OSu (40 mmol) in 40 ml DMF, with 4 ml of NMM added, for 20 hours. The solvent was removed and the residue taken up in 10% HOAc (100 ml). The product was extracted into EtOAc (4 times 100 ml), washed twice with a small volume of H2O, dried over Na2SO4, evaporated to a small volume, and treated with petroleum ether until cloudiness developed. A crystalline product formed on storage in the refrigerator overnight: Yield, 8.2 g (76.3%); mp 115°-118°.

1. customevaporated to dryness
2. customthe oily residue re-evaporated twice with DMF (30 ml each)
3. customThe salt obtained
4. additionadded, for 20 hours
5. customThe solvent was removed
6. extractionThe product was extracted into EtOAc (4 times 100 ml)
7. washwashed twice with a small volume of H2O
8. dry with materialdried over Na2SO4
9. customevaporated to a small volume
10. additiontreated with petroleum ether until cloudiness
11. customA crystalline product formed on storage in the refrigerator overnight
12. customYield