HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 90907901, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,1'-Thiocarbonyldiimidazole | HCID 80264 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Reactant | HCID 72359952 | HCID 72359952 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 90907901 | HCID 90907901 | 52% |
Reaction Steps
To a suspension of 3,4-diamino-N′-[1-{5-(3,4-dichlorophenyl)-4-hydroxythiophen-3-yl}ethylidene]benzohydrazide(30 mg, 0.064 mmol, see the synthetic example 176) in tetrahydrofuran (3.0 mL) was added sodium tert-butoxide (12 mg, 0.13 mmol) and N,N′-thiocarbonyldiimidazole (23 mg, 0.13 mmol). The reaction mixture turned clear orange and was stirred at room temperature for 16 hours, and then was acidified with 1M aqueous HCl solution (1.0 mL) and concentrated under the reduced pressure. The precipitated solid was collected by filtration, washed with chloroform, washed with methanol and dried by means of a vacuum pump to give the desired product as a pale brown solid (yield 52%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07576115B2 |
| Source dataset | uspto-grants-2009_08 |
| ORD ID | ord-2a9b9c67e919425a87cd873050e71742 |
| Source note | uspto-grants-2009_08 |