HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 86752943, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 10752421 | HCID 10752421 | — |
| Reactant | HCID 19068157 | HCID 19068157 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86752943 | HCID 86752943 | — |
Reaction Steps
A stirred solution of 3-7 (142 mg, 0.4 mmol), 2-9 (110 mg, 0.4 mmol), HOBT (61 mg, 0.4 mmol), N(i-Pr)2Et (216 μL, 1.2 mmol) and DMF (7 mL) at -15° C. was treated with EDC (77 mg, 0.4 mmol) followed by removal of the cooling bath. After 20 h. the reaction mixture concentrated followed by dilution with EtOAc. The EtOAc solution was washed with 1M NaHSO4, and brine, dried (MgSO4), and concentrated. Flash chromatography (silica, 10% to 20% acetone/CH2Cl2) to give 3-8 as a viscous gum. Rf 0.64 (silica, 20% acetone/CH2Cl2).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05786373 |
| Source dataset | uspto-grants-1998_07 |
| ORD ID | ord-b3f4d268f50e4a6ebde81f2d924c1219 |
| Source note | uspto-grants-1998_07 |