HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 45092164, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Trimethylsilyldiazomethane | HCID 167693 | — |
| Reactant | HCID 178453125 | HCID 178453125 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 45092164 | HCID 45092164 | — |
Reaction Steps
To a stirred solution of Intermediate 36 (1.0 g) in dichloromethane (35 ml) and methanol (10 ml) at 22° C. under nitrogen was added dropwise 10% trimethylsilyldiazomethane in hexane (12.0 ml). The mixture was stirred for 2 h at 22° C. before acetic acid (2 ml) was added dropwise and the solvents were evaporated in vacuo. The crude residue was purified by Biotage flash column chromatography on silica gel (90 g cartridge), eluting with 10% cyclohexane in ether. The fractions for the first eluting isomer were combined and the solvents evaporated in vacuo to give the title compound as pale yellow crystals (0.487 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07157457B2 |
| Source dataset | uspto-grants-2007_01 |
| ORD ID | ord-27f7ed00f80a407893cbe9d582ebb1e4 |
| Source note | uspto-grants-2007_01 |