HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 54108658, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Pentafluorophenol | HCID 13041 | — |
| Reactant | HCID 23294594 | HCID 23294594 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 54108658 | HCID 54108658 | 56% |
Reaction Steps
To an ice-cooled solution of 5-methyl-3-methylcarbamoyl-hexanoic acid (0.40 g, 2.13 mmol) in dichloromethane (10 ml) was added pentafluorophenol (0.43 g, 2.35 mmol) and EDC (0.45 g, 2.35 mmol). The mixture was stirred at room temperature for 2 h, diluted with more dichloromethane and washed successively with 1 M Na2CO3 solution, 1M HCl and brine. The organic phase was dried (anhydrous MgSO4), filtered and evaporated to leave the title compound as an oil (0.38 g, 56%), which was used in Step D without further purification. 1H-NMR; δ (CDCl3), 5.77 (1H, m), 3.10 (1H, m), 2.83 (3H, d, J=4.7 Hz), 2.75 (2H, m), 1.70 (1H, m), 1.59 (1H, m), 1.31 (1H, m), 0.95 (3H, d, J=4.9 Hz) and 0.93 (3H, d, J=4.8 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05962529 |
| Source dataset | uspto-grants-1999_10 |
| ORD ID | ord-7b58c9761b024a53816ed94eb621b07d |
| Source note | uspto-grants-1999_10 |