HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 22235386, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 22235448 | HCID 22235448 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Ammonium Hydroxide | HCID 14923 | — |
| Product | HCID 22235386 | HCID 22235386 | 71.5% |
Reaction Steps
To a solution of tert-butyl 3-[4-(4-cyanophenyl)-4-(3,4-dimethoxyphenoxy)butyl]-3,8-diazabicyclo[3.2.1]octane-8-carboxylate (17.3 g, 33.2 mmol; from step (a) above) in CH2Cl2 (600 mL) was added TFA (130 mL). The resulting solution was stirred for 30 min then concentrated in vacuo. The residue was neutralized with aqueous Na2CO3, extracted with CH2Cl2 (3×), dried (Na2SO4), filtered and concentrated in vacuo to give an oil. Flash chromatography on silica gel eluting with CH2Cl2:MeOH:concentrated NH4OH (177:20:3) gave 5.0 g (36%) of the title compound as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07012074B2 |
| Source dataset | uspto-grants-2006_03 |
| ORD ID | ord-5f24f3e8c2d649bba5bb6453321d0ac0 |
| Source note | uspto-grants-2006_03 |