HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylenediamine → 4-(2-IMIDAZOLIN-2YL)-7-METHYL-2H,3H,4H-BENZO[e]THIIN
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylenediamine | HCID 3301 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | 7-Methoxy-6-methyl-1,2,3,4-tetrahydronaphthalenecarbonitrile | HCID 67530055 | — |
| Product | 4-(2-IMIDAZOLIN-2YL)-7-METHYL-2H,3H,4H-BENZO[e]THIIN | HCID 67529920 | — |
Reaction Steps
This compound was prepared in a manner analogous to that of Step G of Example 1, by the reaction of 2.0 grams (0.0106 mole) of 7-methyl-2H,3H,4H-benzo[e]thiin-4-carbonitrile (iv) and 6 grams (0.024 mole) of the ethylenediamine salt of p-toluenesulfonic acid (prepared in Step F of Example 1). The reaction product was purified by column chromatography on Grade II alumina (basic-3% water) using a 99:1 mixture of methylene chloride and methanol, respectively, as an eluant. The appropriate fractions of eluate were combined and concentrated under reduced pressure, yielding 1.2 grams of subject compound. The NMR spectrum was consistent with the proposed structure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07417057B2 |
| Source dataset | uspto-grants-2008_08 |
| ORD ID | ord-b515637c508e421baa5d6a8b009a680f |
| Source note | uspto-grants-2008_08 |