HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → HCID 22235338, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| Reactant | HCID 22235399 | HCID 22235399 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Ammonium Hydroxide | HCID 14923 | — |
| Product | HCID 22235338 | HCID 22235338 | 127.2% |
Reaction Steps
To a solution of tert-butyl 3-[3-(4-cyanophenoxy)-2-hydroxypropyl]-3,8-diazabicyclo[3.2.1]octane-8-carboxylate (3.86 g, 9.96 mmol; from step (a) above) in EtOAc (100 mL) was added HCl/EtOAc (150 mL). The resulting solution was stirred for 2 h and concentrated in vacuo to give a foam. The crude product was neutralised with aqueous NaHCO3, extracted with CH2Cl2 (3×), dried (Na2SO4), filtered and concentrated in vacuo. Flash chromatography of the residue on silica gel eluting with CH2Cl2:MeOH:concentrated NH4OH (177:20:3) gave 1.82 g (64%) of the title compound as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07012074B2 |
| Source dataset | uspto-grants-2006_03 |
| ORD ID | ord-f9b81245a1ba4736bc2d0c11f1309cd4 |
| Source note | uspto-grants-2006_03 |