HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 178456090, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | Bis-(1H-imidazol-2-YL)-methanone | HCID 5250894 | — |
| Reactant | HCID 178456092 | HCID 178456092 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 178456090 | HCID 178456090 | 35.2% |
Reaction Steps
To the compound 54 (114 mg) in a methylene chloride (2 ml) solution, carbonyl diimidazole (45 mg) was added, and the mixture was stirred at room temperature for 45 minutes. The reaction solution was cooled to 0° C., then 28% ammonia aqueous solution (2 ml) was added, and the mixture was stirred at that temperature for 1 hour. The reaction solution was diluted with chloroform and the resultant mixture successively washed with water, 1M hydrochloric acid, and brine. The organic layer was dried over anhydrous sodium sulfate, then was concentrated. The residue was purified by flash column chromatography (silica gel, chloroform/ethyl acetate=7/3 to 1/2) to obtain the title compound (40 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846660B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-6b14c3d51b5842f1b2f1a74fefece3e2 |
| Source note | uspto-grants-2014_09 |