HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → {1-Methoxy-6-[(triphenylmethyl)amino]hexylidene}propanedinitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Diazomethane | HCID 9550 | — |
| Reactant | HCID 15406052 | HCID 15406052 | — |
| Solvent | Ethyl ether methylene chloride | HCID 21881112 | — |
| Product | {1-Methoxy-6-[(triphenylmethyl)amino]hexylidene}propanedinitrile | HCID 15406053 | — |
Reaction Steps
A suspension of the malononitrile of Example 2 (13 g, 31 mmole) in ether/dichloromethane (900 mL/100 mL), cooled in an ice bath, was treated with a freshly prepared ethereal solution of diazomethane (from 50 mmole of Diazald® (Aldrich Chemical Company)). The solution was stirred for 6 hr and then neutralized with acetic acid (10 mL). The solution was evaporated to dryness and the residue chromatographed on silica gel using dichloromethane/acetone (4/1) as the eluent. Fractions containing product were pooled and evaporated to a syrup. The syrup was triturated with dichloromethane to induce crystallization. The crystals were filtered and dried to give 8.3 g (61%) of chromatographically pure product, useful as an intermediate compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05824796 |
| Source dataset | uspto-grants-1998_10 |
| ORD ID | ord-7315e7a2232243cfa7b0ebb109a46106 |
| Source note | uspto-grants-1998_10 |