HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68290887, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 88924193 | HCID 88924193 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68290887 | HCID 68290887 | 81% |
Reaction Steps
To 1-(8-ethyl-10,10-dimethyl-11-oxa-3,8-diazaspiro[5.5]undecan-3-yl)-2,2,2-trifluoro-ethanone hydrochloride salt (47 mg, 0.14 mmol) and lithium hydroxide (10 mg, 0.42 mmol) was added water (0.15 mL) and THF (0.6 mL) and the reaction mixture was stirred at room temperature for 2 hours. The reaction mixture was concentrated in vacuo, partitioned between DCM (10 mL)/1:1 brine:NH4OH (2 mL), extracted with DCM (5×10 mL), dried over MgSO4 and concentrated in vacuo to give 4-ethyl-2,2-dimethyl-1-oxa-4,9-diazaspiro[5.5]undecane (24 mg, 81%). ESI-MS m/z calc. 212.2. found 213.5 (M+1)+; Retention time: 0.19 minutes (3 min run).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09181273B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-ba02b63bf5e04bedac07cab0c4892522 |
| Source note | uspto-grants-2015_11 |