HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → 2,6-Bis(4-cyanophenoxy)-nicotinic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 67606024 | HCID 67606024 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2,6-Bis(4-cyanophenoxy)-nicotinic acid | HCID 67605998 | — |
Reaction Steps
0.2 g (8.4 mmol) of lithium hydroxide was added to a stirred solution of 2,6-bis(4-cyano phenoxy)-nicotinic acid ethyl ester, 1.6 g (4.15 mmol), in a mixture of 5 ml of water and 2.5 ml of THF (2:1) at 5° C. and the contents were stirred for 3 h at RT. The reaction mixture was washed with diethylether. 6 N HCl was added to aqueous layer with stirring until the solution attained a pH of 2. The white precipitate obtained was collected, washed with water and dried under reduced pressure to afford 1.1 g of the required product. Percentage purity (LCMS): 83.2%, (M+1)=357.0+1. 1H NMR (DMSO-d6): δ 6.98 (1H, d), 7.26 (4H, d), 7.80 (4H, d), 13.22 (1H, brs).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08722930B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-e5323bec0c614453a9d0fdc925bc7143 |
| Source note | uspto-grants-2014_05 |