HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodoethane → HCID 46219099, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodoethane | HCID 6340 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 46196348 | HCID 46196348 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 46219099 | HCID 46219099 | 35.9% |
Reaction Steps
Preparation according to Example 2. (+3-(3-chloro-2-fluorophenyl)-3-methoxypyrrolidine (0.234 g, 1.02 mmol), tetrahydrofuran (20 ml), iodoethane (0.122 ml, 1.15 mmol) and triethylamine (0.285 ml, 2.04 mmol), the solution was stirred for 26 h. Purification by HPLC on waters OBD C18, 5 μm (MeOH/33 mM NH3, 20:80 to 65:35) gave the title compound 0.094 g (35.9%). [a]D=−16.1° (methanol). The amine was converted to the fumaric acid salt and recrystallized from 2-propanol/diisopropyl ether: M.p. 131-133° C. MS m/z (rel. intensity, 70 eV) 257 (M+, 4), 242 (38), 227 (20), 157 (31), 71 (bp).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09035073B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-f471ab48424e4678a446d8ab58ce4be8 |
| Source note | uspto-grants-2015_05 |