HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → HCID 89648817, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | HCID 89649733 | HCID 89649733 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 89648817 | HCID 89648817 | — |
Reaction Steps
To a solution of (2R,5S)-7-methyl-2-[4-[4-(trifluoromethyl)phenyl]-2-pyridyl]-1,7-diazaspiro[4.4]nonan-6-one hydrochloride (which may be prepared as described in Example 52) (21 mg, 0.0500 mmol) in methanol (0.5000 mL) was added 3 meq of 3.7% formalin solution and sodium triacetoxyborohydride (16.21 mg, 0.0800 mmol) and the mixture was stirred for 1 h. The mixture was evaporated and partitioned between satd. aq. NaHCO3 (2 ml) and MDC (3×5 ml) and the residue purified on an SCX-2 cartridge (0.5 g) eluting with MeOH to 2% aq NH3 in MeOH to give (2R,5S)-1,7-dimethyl-2-[4-[4-(trifluoromethyl)phenyl]-2-pyridyl]-1,7-diazaspiro[4.4]nonan-6-one, a clear oil (16.9 mg);
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09376436B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-60616a9d03d9469bb9d89459300e7956 |
| Source note | uspto-grants-2016_06 |