HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylmorpholine → HCID 19385750, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | Isobutyl chloroformate | HCID 62365 | — |
| Reactant | HCID 18973695 | HCID 18973695 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | HCID 19385750 | HCID 19385750 | 92.1% |
Reaction Steps
A mixture of 2-carboxy-4-cyano-4-(3-cyclopropylmethoxy-4-methoxyphenyl)-1-(methoxymethyloxy)cyclohex-1-ene (0.26 g. 0.67 mmol), N-methyl morpholine (0.09 ml, 0.8 mmol) and isobutyl chloroformate (0.1 mL, 0.77 mmol) in dry 1,2-dimethoxyethane (7 mL) was stirred under an argon atmosphere at room temperature for 10 min. Ammonium hydroxide (0.07 mL, 1.0 mmol) was added and stirring was continued for 0.5 h. The mixture was partitioned between methylene chloride and 5% aqueous sodium carbonate, was extracted three times, the organic layer was dried (potassium carbonate) and the solvent was removed in vacuo to provide a white solid (0.22 g, 85%): m.p. 120°-122° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05449686 |
| Source dataset | uspto-grants-1995_09 |
| ORD ID | ord-556c818357c444ba920fe73af9e5c96d |
| Source note | uspto-grants-1995_09 |