HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bis(2,2,2-trichloroethyl) hydrazine-1,2-dicarboxylate → Bis(2,2,2-trichloroethyl) 1-(2,3-dihydrobenzofuran-5-yl)hydrazine-1,2-dicarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bis(2,2,2-trichloroethyl) hydrazine-1,2-dicarboxylate | HCID 350435 | — |
| Reactant | Bis(2,2,2-trichloroethyl) 1-(2,3-dihydrobenzofuran-5-yl)hydrazine-1,2-dicarboxylate 2,3-Dihydro-benzofuran | HCID 86648897 | — |
| Catalyst | Zincchloride | HCID 3007855 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Bis(2,2,2-trichloroethyl) 1-(2,3-dihydrobenzofuran-5-yl)hydrazine-1,2-dicarboxylate | HCID 10505571 | 96.6% |
Reaction Steps
Bis(2,2,2-trichloroethyl) 1-(2,3-dihydrobenzofuran-5-yl)hydrazine-1,2-dicarboxylate 2,3-Dihydro-benzofuran 7a (0.6 mL, 5.32 mmol), bis(2,2,2-trichloroethyl) hydrazine-1,2-dicarboxylate (1.96 g, 5.15 mmol) and zinc chloride (920 mg, 6.76 mmol) were dissolved in 40 mL of dichloromethane. The reaction was reacted overnight at room temperature and monitored by TLC until the disappearance of the starting materials. Then the mixture was purified by silica gel column chromatography to obtain the title compound bis(2,2,2-trichloroethyl) 1-(2,3-dihydrobenzofuran-5-yl)hydrazine-1,2-dicarboxylate 7b (2.5 g, yield 96.6%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08367710B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-3a13d733d8684b419f183f2627834bef |
| Source note | uspto-grants-2013_02 |