HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 66727319, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | HCID 66726990 | HCID 66726990 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 66727319 | HCID 66727319 | — |
Reaction Steps
0.2 mL of triethylamine and 0.1 mL of ethyl chlorocarbonate were added dropwise with stirring at 0° C. to a methanol (5 mL) solution of 300 mg of 6-(4-tert-butoxycarbonyl-1,4-diazepan-1-ylsulfonyl)isoquinoline 2-oxide, and the mixture was then stirred at room temperature for 3 hours. After the completion of reaction, the reaction solvent was distilled off under reduced pressure. To the obtained residue, 20 mL of ethyl acetate was added, and the deposited insoluble matter was removed by filtration. The filtrate was concentrated, and the obtained crude product was purified by silica gel column chromatography (ethyl acetate:hexane=1:1) to obtain 110 mg of the compound of interest as a white crystal (36%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08951997B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-d9a2b0ae18264695878dac50da085558 |
| Source note | uspto-grants-2015_02 |