HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → HCID 178500939, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Dimethyl acetylenedicarboxylate | HCID 12980 | — |
| Reactant | HCID 178526316 | HCID 178526316 | — |
| Product | HCID 178500939 | HCID 178500939 | — |
| Product | HCID 178500940 | HCID 178500940 | — |
Reaction Steps
To a suspension of azepan-2-one oxime in acetonitrile 1.1 eq. of dimethyl acetylenedicarboxylate were added dropwise under stirring. The mixture was stirred at room temperature for 1 hour. The solvent was removed under reduced pressure to afford a mixture 8/1 of dimethyl (2E)-2-[(azepan-2-ylideneamino)oxy]but-2-enedioate and dimethyl (2Z)-2-[(azepan-2-ylideneamino)oxy]but-2-enedioate as a yellow oil. To better characterize the title compounds a small amount of the crude was purified by preparative RP-HPLC, using water (0.1% TFA) and acetonitrile (0.1% TFA) as eluents (column C1-8). The pooled product fractions were lyophilized.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07968553B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-9a6b5e3e40aa48feaaac52e29ececec1 |
| Source note | uspto-grants-2011_06 |