Table 4.
Procedure | Reagents | Volume/Time |
---|---|---|
H-Phosphonate/H-Phosphinate Condensation Step | ||
Deblocking | 3% DCA in DCM | Flow through the column 6 mL/2 min |
Condensation | 0.1M monomer in ACN/Py (1:1) | 120 µL/10min |
0.3M DMOCP in ACN/Py (95:5) | ||
Oxidation | Ox-A, Ox-B, Ox-D | 220 µL/30 min |
Methyl-ester cleavage * | PhSH/Et3N/DMF(1:1.4:2) | 300 µL/4 h |
Cleavage from solid support | Gaseous ammonia at 0.7 MPa | Gas chamber/16 h |
* Applicable only in case of Ox-A and Ox-B mixtures containing methanol.