HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 86690951, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | HCID 86690950 | HCID 86690950 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86690951 | HCID 86690951 | — |
Reaction Steps
208 mg (0.36 mmol) of the compound from Example 141 were initially charged in 5 ml of DMF, and 62 mg (0.46 mmol) of HOBt and 88 mg (0.46 mmol) of EDC were added. After 10 min of stirring at RT, 1.0 ml (16 mmol) of ammonia solution (33% strength in water) were added, and the mixture was stirred at RT for 16 h. Under reduced pressure, the reaction solution was then freed from excess ammonia, about 3 ml of water were added and the mixture was extracted three times with in each case 5 ml of ethyl acetate. The combined organic phases were dried over magnesium sulfate, filtered and concentrated under reduced pressure. The crude product was purified chromatographically [Method 19]. This gave 85 mg (39% of theory) of the target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09187466B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-89ad313c2157456a9666cbbf198f6786 |
| Source note | uspto-grants-2015_11 |