HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 117610599, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | Ethyl 2-(4,5-dichloro-2-hydroxyphenylamino)acetate | HCID 117610965 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 117610599 | HCID 117610599 | 111.5% |
Reaction Steps
To a solution of ethyl 2-((4,5-dichloro-2-hydroxyphenyl)amino)acetate (2 g, 7.6 mmol) in of 4:1 mixture of tetrahydrofuran and water (30 mL) at room temperature, LiOH.H2O (3.2 g, 76 mmol) were added and the resulting mixture was stirred for 30 min and then acidified with aqueous HCl (1N) to adjust the pH to 3-5. The mixture was extracted with ethyl acetate (40 mL×3). The combined organic layer was washed with brine (40 mL×3), dried over anhydrous Na2SO4, filtered and concentrated in vacuo to afford the crude product (2 g) which was used directly in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09227978B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-37edc36115b947c481bdec83ebf19cca |
| Source note | uspto-grants-2016_01 |