Table 1.
| ||
---|---|---|
entry | conditionsa | yieldb |
1 | 1.2 equiv Z-Leu-OH, 1.2 equiv HBTU, HOBt, NEt3, MeCN | trace |
2 | 1.2 equiv Z-Leu-OH, 1.2 equiv PyBOP, NEt3, DMF | trace |
3 | 1.2 equiv Z-Leu-OH, 1.2 equiv EDC, HOBt, NEt3, DCM | trace |
4 | 1.2 equiv Z-Leu-OH, 1.2 equiv EDC, 0.2 eq. DMAP, DCM | 33c |
5 | 2.0 equiv Z-Leu-OH, 2.0 equiv EDC, 0.2 eq. DMAP, DCM | 58c |
6 | 1.2 equiv Z-Leu-OH, 1.2 equiv EDC, DCM | 59 |
7 | 2.0 equiv Z-Leu-OH, 2.0 equiv EDC, DCM | 91 |
8 | 2.0 equiv Z-Leu-OH, 2.0 equiv PyBOP, DCM | 33 |
9 | 2.0 equiv Z-Leu-OH, 2.0 equiv COMU, DCM | 44 |
10 | 2.0 equiv Z-Leu-OH, 2.0 equiv DEPBT, DCM | 26 |
11 | 2.0 equiv Z-Leu-OH, 2.0 equiv DCC, DCM | 77 |
All reactions carried out for 24 h at rt.
Isolated yields.
HPLC analysis of a phenylalanyl derivitive showed significant epimerization of the Leu chiral center.