HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 178484843, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 178418329 | HCID 178418329 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178484843 | HCID 178484843 | 89% |
Reaction Steps
To a mixture of lithium aluminium hydride (9 g, 0.23 mol) in tetrahydrofuran (425 mL) was added slowly tert-butyl (trans-4-hydroxycyclohexyl)carbamate (intermediate 1, 10 g, 0.046 mol). The mixture was refluxed overnight. Once the mixture was cooled to room temperature, 9 ml of water, 9 ml of 4N NaOH solution and 18 ml of water were carefully and successively dropped. The organic solvent was removed under reduced pressure and the crude obtained was dissolved with chloroform and dried over magnesium sulphate. The filtrate was evaporated to dryness and co evaporated with hexane to give the title compound as a white solid (89%). This intermediate is also described in JMC, 1987, 30(2), p 313.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09233108B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-41e511a820cf49698d5b30af83656bec |
| Source note | uspto-grants-2016_01 |