HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 178527033, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Diethylphosphite | HCID 3780918 | — |
| Reactant | HCID 178419670 | HCID 178419670 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 178527033 | HCID 178527033 | 66.7% |
Reaction Steps
To a solution of 25 mmol of (2-phenyl)ethylmagnesium bromide in 25 ml of diethyl ether was added dropwise with cooling (ice bath) 0.92 ml (7.14 mmol) of diethyl phosphite. The resulting solution was heated at reflux for 2 h, cooled, and treated with aqueous ammonium chloride. The product was extracted with ether, dried over MgSO4, and concentrated in vacuo. Flash chromatography using ethyl acetate gave 1.23 g (64%) of the desired compound (Rf 0.64, 10% methanol in chloroform) as a colorless oil. 1H NMR (CDCl3) δ 2.0-2.2 (m, 4H), 2.85-3.1 (m, 4H), 6.89 (dm, J=455 Hz, 1H), 7.15-7.4 (m, 10H). Mass spectrum (M+H)+ =259.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05670675 |
| Source dataset | uspto-grants-1997_09 |
| ORD ID | ord-a0c9bb99fc2d455bb1d9ac254f44f5a3 |
| Source note | uspto-grants-1997_09 |