HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → (S)-1-((R)-2,3-Dihydrobenzo[1,4]dioxine-2-carbonyl)-3-methylpiperidine-3-carboxylic acid ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | (R)-2,3-Dihydrobenzo[1,4]dioxine-2-carbonyl chloride | HCID 7022160 | — |
| Reactant | (S)-Ethyl 3-methylpiperidine-3-carboxylate | HCID 23389262 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (S)-1-((R)-2,3-Dihydrobenzo[1,4]dioxine-2-carbonyl)-3-methylpiperidine-3-carboxylic acid ethyl ester | HCID 66727067 | 99.2% |
Reaction Conditions
| Temperature | 5 °C |
|---|
Reaction Steps
(R)-2,3-Dihydrobenzo[1,4]dioxine-2-carbonyl chloride (6.05 g, 30.5 mmol) in DCM (20 ml) was added to a stirred mixture of (S)-3-methyl-piperidine-3-carboxylic acid ethyl ester (5.0 g, 29.2 mmol), DIPEA (5.5 ml, 31.7 mmol) and DCM (30 ml), previously cooled down to 5° C. The cooling bath was removed and stirring continued at RT for 1 h. The reaction mixture was washed twice with 1 M HCl, twice with sat. aq NaHCO3 and twice with water and dried with Na2SO4. Solvent was evaporated to give 9.66 g of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08492549B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-e9b963cb36f2417cab6cb8a8354a578d |
| Source note | uspto-grants-2013_07 |