HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylamine → (+/-)-3-[2,4-Bis(methoxymethoxy)phenyl]-N-ethylcyclohexanecarboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylamine | HCID 6341 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Isobutyl chloroformate | HCID 62365 | — |
| Reactant | (+/-)-3-[2,4-Bis(methoxymethoxy)phenyl]cyclohexanecarboxylic Acid | HCID 22337771 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (+/-)-3-[2,4-Bis(methoxymethoxy)phenyl]-N-ethylcyclohexanecarboxamide | HCID 22337779 | — |
Reaction Steps
Triethylamine (11 μl) and isobutylchloroformate (10 μl) were added to a stirred solution of (±)-3-[2,4-bis(methoxymethoxy)phenyl]cyclohexanecarboxylic acid in anhydrous tetrahydrofuran (2 ml) under argon at 0° C. After 30 min, ethylamine (0.5 ml, 2M solution in tetrahydrofuran) was added. The reaction mixture was partitioned between water (20 ml) and ethyl acetate (50 ml). The aqueous layer was extracted with ethyl acetate (2×20 ml) and the combined organic extracts were dried over magnesium sulfate and evaporated in vacuo to give the title compound as a solid (24 mg, quant.) and a mixture of diastereoisomers; m/z (ES+) 352 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06828460B2 |
| Source dataset | uspto-grants-2004_12 |
| ORD ID | ord-69c3855625b44badbda39524cbb267b1 |
| Source note | uspto-grants-2004_12 |