HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodoethane → HCID 15157487, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodoethane | HCID 6340 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | HCID 15157460 | HCID 15157460 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 15157487 | HCID 15157487 | — |
Reaction Steps
To a solution of the titled product of Example 43 (676 mg, 1.25 mmol) in 5 ml of dimethylformamide (DMF) was added 190 mg (1.25 mmol) of 1,8-diazabicyclo (5.4.0)undec-7-ene followed by 585 mg (3.75 mmol) of iodoethane. After stirring overnight at room temperature, the solvent was removed under reduced pressure. The residue was dissolved in CH2Cl2. The solution was then washed with 3N hydrochloric acid, dried (Na2SO4), filtered, and the solvent removed on a rotary evaporator. The residue was chromatographed on a silica gel column. Elution with 35% ethyl acetate/61.5% hexane/2.5% acetic acid as eluent produced the title product which was crystallized from 3:1 hexane:ethyl acetate to give 183 mg, m.p. 83.5°-84.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05093353 |
| Source dataset | uspto-grants-1992_03 |
| ORD ID | ord-562def7eee674ae7913c32c032b230c0 |
| Source note | uspto-grants-1992_03 |