HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 67517832, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Sodium Formate | HCID 2723810 | — |
| Reactant | HCID 86702735 | HCID 86702735 | — |
| Solvent | Formic Acid | HCID 284 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67517832 | HCID 67517832 | — |
Reaction Steps
0.91 g (2.30 mmol) of 2-(2,6-diethyl-4-methylphenyl)-5-formyl-3-oxooctahydropentalen-1-yl 2,2-dimethylpropanoate (Example I-b-2), 0.78 g (11.48 mmol) of sodium formate and 0.80 g (11.48 mmol) of hydroxylamine hydrochloride in 30 ml of formic acid are heated at reflux for 72 h. 50 ml of water are then added, and the mixture is stirred at room temperature for 1 h, taken up in ethyl acetate, washed twice with water, dried (magnesium sulphate) and concentrated using a rotary evaporator. The residue is chromatographed on silica gel (mobile phase ethyl acetate/hexane 1:6). This gives 0.31 g (44%) of the desired compound as a colourless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09101133B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-fa551dfb510142d18912a99523380234 |
| Source note | uspto-grants-2015_08 |