Table 3.
ArX | Pd Sourcea,b | Ligandc,d | Basee,f | Solventg | Temp. (°C)/Time (h) | Results | |
---|---|---|---|---|---|---|---|
1 | 36a | Pd(OAc)2 | DCPB | K3PO4 | dioxane:H2O | 100/24 | 35 + 36a |
2 | 37a | Pd(OAc)2 | DCPB | K3PO4 | dioxane:H2O | 100/24 | 35 + 37a |
3 | 36a | Pd(OAc)2 | DCPB | CsF | dioxane | 100/24 | 35 + 36a |
4 | 36a | Pd(OAc)2 | XPhos | K3PO4 | Tol:H2O | 100/24 | 35 + 36a |
5 | 36a | Pd(OAc)2 | DavePhos | K3PO4 | Tol:H2O | 100/24 | 35 + 36a |
6 | 36a | Pd(OAc)2 | SPhos | K3PO4 | Tol:H2O | 100/24 | 35 + 36a |
7 | 36a | Pd(OAc)2 | SPhos | K3PO4 | THF:H2O | 50/24 | 38a (20%)+38b (10%) + 35 (15%) + 36a (13%) |
8 | 36a | Pd(OAc)2 | SPhos | K3PO4 | THF:H2O | 50/48 | 38a (37%) + 38b (18%) + 35 (20%) |
9 | 36a | Pd2(dba)3 | SPhos | K3PO4 | THF:H2O | 50/48 | 38a (38%) + 38b (19%) + 35 (20%) |
5 mo % of Pd(OAc)2;
2.5 mol % of Pd2(dba)3;
Ligands: DCPB: 2-(Dicyclohexylphosphanyl)biphenyl; XPhos: 2-Dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl; DavePhos: 2-Dicyclohexylphosphino-2′-(N,N-dimethylamino)biphenyl; SPhos: 2-Dicyclohexylphosphino-2′6′-dimethoxybiphenyl;
20 mol % of ligand;
2 equiv. of K3PO4;
8 equiv. of CsF;
solvent:H2O/10:1.