HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 71187300, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 71186642 | HCID 71186642 | — |
| Solvent | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| Product | HCID 71187300 | HCID 71187300 | 37.5% |
Reaction Steps
6-tert-butyl 5-methyl 5-methyl-6-azaspiro[2.5]octane-5,6-dicarboxylate (D5) (320 mg, 1.13 mmol) was partitioned between dioxane/water (8/8 ml) prior addition of LiOH H2O (190 mg, 4.52 mmol). The mixture was stirred at RT for 18 hrs then heated at 150° C. under microwave irradiation 40 min (4 cycles of 10 min each). Organic solvent was evaporated off and the aqueous solution washed with EtOAc (2×10 ml), acidified to pH˜4 with citric acid sat. sol. and extracted with EtOAc (3×10 ml). The organic phases were washed with NaCl sat. sol, dried over Na2SO4 and evaporated to reduced pressure to afford the title compound (D6) (114 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09181279B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-bffa82e3c3404c76b4a6e72d3c98d0c6 |
| Source note | uspto-grants-2015_11 |