Table 1.
Iridium‐catalyzed hydroxymethylation of 1 a.
|
| ||||
|---|---|---|---|---|
|
Entry |
Paraformaldehyde (equiv) |
KI (equiv) |
T [°C] |
Yield [%] |
|
1 |
20 |
4 |
65 |
65 |
|
2 |
20 |
4 |
45 |
66 |
|
3 |
20 |
2 |
45 |
66 |
|
4[a] |
20 |
2 |
45 |
0 |
|
5 |
25 |
2 |
45 |
71 |
|
6 |
30 |
2 |
45 |
73 |
|
7 |
40 |
2 |
45 |
63 |
|
8[b] |
30 |
2 |
45 |
73 |
|
9 |
30 |
2 |
25 |
76 |
|
10[c] |
30 |
2 |
45 |
0 |
[a] Using NaOMe (1.5 equiv) as base. [b] Using 1.5 equiv of Mg(OMe)2. [c] With no iridium.