HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diazomethane → HCID 53955469, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diazomethane | HCID 9550 | — |
| Reactant | HCID 22850672 | HCID 22850672 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 53955469 | HCID 53955469 | — |
Reaction Steps
A solution of 368 mg (0.725 mmole) of (S)-4-(dipentylcarbamoyl)-1-(diphenylacetyl)piperazine-2-carboxylic acid (from Example 9) in 5 ml of methanol was treated at 0° C. with 20 ml of diazomethane solution in diethyl ether (prepared by the procedure above). The solution was strirred at 0° C. for 30 minutes and at 25° C. for 30 minutes. The excess diazomethane was destroyed by the dropwise addition of acetic acid until the solution became colorless. The resulting solution was concentrated in vacuo and the residue was chromatographed over an 85×2.5 cm LH-20 column and concentrated in vacuo to 225 mg (59%) of pale colored oil which was homogeneous by TLC (1:1 hexane-ethyl acetate, Rf =0.7).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05292726 |
| Source dataset | uspto-grants-1994_03 |
| ORD ID | ord-c27a1cb483f9464098d7f2614b354878 |
| Source note | uspto-grants-1994_03 |