HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 88929351, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | 1485347-75-8 | HCID 78929116 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 88929351 | HCID 88929351 | 103% |
Reaction Steps
A mixture of 4-(trifluoromethoxy)butanoic acid (1.0 g, 5.81 mmol) and HOBt (1.157 g, 7.55 mmol) in MeCN (20 mL) was treated with EDC (1.448 g, 7.55 mmol) and stirred at RT for 2 h. Ammonium hydroxide (˜15M, 0.7 mL, ˜10.5 mmol) was added and the mixture stirred at RT for 20 h. The mixture was treated with Et2O, water and brine, the layers separated and the organic layer dried over Na2SO4 and concentrated to afford 4-(trifluoromethoxy)butanamide (1.024 g, 103%) as a white solid. 1H NMR (400 MHz, DMSO-d6): δ 7.30 (s, 1H), 6.78 (s, 1H), 4.04 (t, J=6.4 Hz, 2H), 2.13 (t, J=7.4 Hz, 2H), 1.82 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09382228B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-68f874f477ff43eebb3b60cc2bb42485 |
| Source note | uspto-grants-2016_07 |