HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 66631775, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 66631685 | HCID 66631685 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66631775 | HCID 66631775 | — |
Reaction Steps
68 mg (0.15 mmol) of 3-{[(3,5-dicyano-6-{[(2R)-2,3-dihydroxypropyl]amino}-4-phenylpyridin-2-yl)sulfanyl]methyl}benzenecarboxylic acid Example 23 were dissolved in 3.4 ml of DMF. After addition of 42.5 mg (0.22 mmol) of EDC and 29.9 mg (0.22 mmol) of HOBT, the mixture was stirred at RT for 10 min. 39.5 mg (0.74 mmol) of ammonium chloride and 133.6 mg (1.03 mmol) of N,N-diisopropylethylamine were added, and the reaction mixture was stirred at RT overnight. Water and tetrahydrofuran were added to the reaction mixture until a clear solution had formed. The solution was purified by preparative HPLC (Chromasil, water/acetonitrile+0.1% trifluoroacetic acid).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09187428B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-43f16369431a43539535d9f6d0298642 |
| Source note | uspto-grants-2015_11 |