HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 43554923, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 43554841 | HCID 43554841 | — |
| Catalyst | Titanium isopropoxide | HCID 11026 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 43554923 | HCID 43554923 | — |
Reaction Steps
To a mixture of 4-(3,4-difluorophenoxy)-3-fluorobenzaldehyde (300 mg, 1.19 mmol) and 7 M NH3 in MeOH (10 mL) was added titanium isopropoxide (0.712 mL, 2.38 mmol). The reaction mixture was stirred overnight at rt. Then, NaBH4 (54.0 mg, 1.43 mmol) was added in portions. The mixture was stirred at rt for 4 h, and quenched with water and filtered. The organic part was extracted with ethyl acetate. Combined organic portions were dried over Na2SO4, filtered and concentrated. Purification via Biotage reverse phase chromatography (acetonitrile/water, 5%-95% with 0.25% TFA) afforded the title product (100 mg) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08975400B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-c61ba789dfe54c20bc92264a59369810 |
| Source note | uspto-grants-2015_03 |