HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 11695946, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 66722385 | HCID 66722385 | — |
| Product | HCID 11695946 | HCID 11695946 | — |
Reaction Steps
To a solution of 2-cyclohexyl-2,7-diazaspiro[4.5]decan-1-one hydrochloride (20 mg, 0.00007 mol) in methylene chloride (0.5 mL, 0.008 mol) was added N,N-diisopropylethylamine (14.0 μL, 0.0000806 mol) and the solution was stirred at rt for 5 min. prior to the addition of N,N-carbonyldiimidazole (24 mg, 0.00015 mol). After stirring the reaction mixture at rt for 3 h, piperidine (6.2 mg, 0.00007 mol) was added and stirring was continued for 12 h. To drive the reaction to completion the mixture was heated at 170° C. under microwave irradiation for 1 h. The crude mixture was purified by prep.-HPLC to afford the desired product. LC-MS: 348.2 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08563570B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-4200b9d5256d42cdb513043e6668c3ef |
| Source note | uspto-grants-2013_10 |