HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 67182634, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 3-Bromo-4-(4-trifluoromethyl-benzyl)-4H-thieno[3,2-b]pyrrole | HCID 58297672 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethyl sulfoxide methanol | HCID 22036561 | — |
| Product | HCID 67182634 | HCID 67182634 | — |
Reaction Steps
A mixture of 2.0 g of the product of Step 5, 0.54 g of PdCl2dppf.CH2Cl2, and 1.8 ml of Et3N in 60 ml of 2:1 DMSO/MeOH was heated under CO (balloon pressure) at 75° C. for 24 h. The reaction mixture was poured into 400 ml of 1:1 heaxan/EtOAc and stirred with 200 ml of water for 4 h. The organic layer was washed with 100 ml of brine and dried over Na2SO4, filtered, and concentrated. The residue was purified by silica gel chromatography eluted with a gradient up to 15% EtOAc/hexane to give 1.7 g of the title compound as a light brown solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08404736B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-d118a30cda904dfca9b240e7ad35fcf0 |
| Source note | uspto-grants-2013_03 |