HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 69001045, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| Reactant | HCID 68999942 | HCID 68999942 | — |
| Reactant | HCID 69002709 | HCID 69002709 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 69001045 | HCID 69001045 | 38% |
Reaction Steps
To a solution of (E)-2-{2-[2-(1H-indazol-3-yl)vinyl]phenylcarbamoyl}nicotinic acid or (E)-3-{2-[2-(1H-indazol-3-yl)vinyl]phenylcarbamoyl}pyridine-2-carboxylic acid (20 mg, 0.052 mmol) obtained in Step 1 in THF (1.0 mL), 1-hydroxybenzotriazole monohydrate (1.6 mg, 0.010 mmol) and EDC (15 mg, 0.078 mmol) were added, followed by heating under reflux for 30 minutes. The reaction mixture was added with water, extracted with ethyl acetate and the organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform to chloroform/methanol=90/10), crystallized from DMF/water (1/1) to obtain Compound 205 (7.2 mg, 38%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07605272B2 |
| Source dataset | uspto-grants-2009_10 |
| ORD ID | ord-abcf9d959ee247a3af0a3aa24cd2a242 |
| Source note | uspto-grants-2009_10 |