HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 136106406, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | HCID 136339726 | HCID 136339726 | — |
| Reactant | HCID 178419017 | HCID 178419017 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 136106406 | HCID 136106406 | 53% |
Reaction Steps
Et3N (0.079 mL, 0.568 mmol, 8.0 eq.) was added to a mixture containing the crude carboxylic acid salt 9c (0.071 mmol, 1.0 eq.), histamine.2HCl (16 mg, 0.085 mmol, 1.2 eq.), EDC (15 mg, 0.078 mmol, 1.1 eq.) and HOBt (11 mg, 0.078 mmol, 1.1 eq.) in dry DMF (2 mL) and stirred for 16 h. The reaction mixture was concentrated in vacuo and the residue was purified by flash chromatography [10% (5% aq NH4OH/MeOH)/DCM] to afford the title compound (Rf=0.40) as a light yellow powder (20.1 mg, 53%). ES-MS MH+ 530.30.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08629147B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-e6d6cee215d546ad86e63a56ef1b0588 |
| Source note | uspto-grants-2014_01 |