Table 2.
| |||
---|---|---|---|
entry | solvent | 2nd base | assay yield |
1 | CH2Cl2 | TEA | 50% |
2 | CH2Cl2 | pyridine | 57% |
3 | CH2Cl2 | 2,4,6-collidine | 84% |
4 | CH2Cl2 | 2,6-lutidine | 80% |
5 | CH2Cl2 | Hünig base | 58% |
6 | CH2Cl2 | N-methyl morpholine | 72% |
7 | CH2Cl2 | dimethylaniline | 69% |
8 | MeCN | 2,4,6-collidine | 97% |
9 | MTBE | 2,4,6-collidine | 87% |
10 | THF | 2,4,6-collidine | 92% |
11 | IPAC | 2,4,6-collidine | 50% |
12 | 2-MeTHF | 2,4,6-collidine | 75% |