HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 118223428, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Cyanogen Bromide | HCID 10476 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 90020746 | HCID 90020746 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 118223428 | HCID 118223428 | 71.7% |
Reaction Steps
Add sodium bicarbonate (270 mg, 3.21 mmol) and cyanogen bromide (187 mg, 1.76 mmol) to the solution of 3-amino-5-(trifluoromethyl)benzohydrazide (400 mg, 1.6 mmol) in ethanol (5 mL), reflux for 5 hrs. TLC (PE:EtOAc=1:1) shows the reaction is complete. Concentrate the mixture, partition the residue between EtOAc and water, collect the organic layer, wash with saturated sodium bicarbonate solution, dry over anhydrous sodium sulfate, and concentrate under reduced pressure to afford the crude product. Recrystallization in ethyl acetate yields the pure product (280 mg, 63%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09359338B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-96963abb2ab34beb9428dc1edc53f95a |
| Source note | uspto-grants-2016_06 |