HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 88569887, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | HCID 56932660 | HCID 56932660 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 88569887 | HCID 88569887 | — |
Reaction Steps
A mixture of 31 mg (47 μmol) of the compound of Example 21, 13 mg (70 μmol) of EDC and 9.4 mg (70 μmol) of HOBt in 2 ml of DMF was stirred at RT for 20 min and then poured into 2 ml of ammonia (35% strength solution in water). The reaction mixture was stirred at RT for 30 min, then briefly concentrated on a rotary evaporator, acidified with 1N hydrochloric acid and separated by preparative HPLC [Method 6]. The appropriate fraction was concentrated on a rotary evaporator and the residue was dried under high vacuum. This gave 29 mg (92% of theory) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09034855B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-58aea20848194019858b9ead35e228f8 |
| Source note | uspto-grants-2015_05 |