HuagongsheHuagongshe Chemistry Print Report · For research reference only
Isobutyl chloroformate → 3-[[5-(Azidomethyl)tetrahydro-3-furanyl]thio]-4-methyl-6-[1-[[(2-methylpropoxy)carbonyl]oxy]ethyl]-7-oxo-1-azabicyclo[3.2.0]hept-2-ene-2-carboxylic acid (4-nitrophenyl)methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Isobutyl chloroformate | HCID 62365 | — |
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Reactant | 3-[[5-(Azidomethyl)tetrahydro-3-furanyl]thio]-6-(1-Hydroxyethyl)-4-methyl-7-oxo-1-azabicyclo[3.2.0]hept-2-ene-2-carboxylic acid (4-nitrophenyl)methyl ester | HCID 86750323 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3-[[5-(Azidomethyl)tetrahydro-3-furanyl]thio]-4-methyl-6-[1-[[(2-methylpropoxy)carbonyl]oxy]ethyl]-7-oxo-1-azabicyclo[3.2.0]hept-2-ene-2-carboxylic acid (4-nitrophenyl)methyl ester | HCID 53659855 | — |
Reaction Conditions
| Temperature | -78 °C |
|---|
Reaction Steps
Using anhydrous conditions, 1.25 g of product from Example 45 in 27 ml of anhydrous tetrahydrofuran, is cooled to -78° C. under argon. 0.325 ml of isobutyl chloroformate is added, followed by 2.7 ml of lithium bis(trimethylsilyl)amide. The reaction mixture is stirred at -78° C. for 1 hour, followed by stirring at -55° C. for another hour and then concentrated in vacuo. The residue is purified by chromatography (Silica Gel: 50% ethyl acetate/hexane) to give 1.22 g of the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05750735 |
| Source dataset | uspto-grants-1998_05 |
| ORD ID | ord-27f0b3e3e0c94ac89d8edda82af489d5 |
| Source note | uspto-grants-1998_05 |