HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Methylbutanal → HCID 57277639, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Methylbutanal | HCID 11552 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | HCID 10697309 | HCID 10697309 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 57277639 | HCID 57277639 | 169.3% |
Reaction Steps
(S)-Azepane-1-carboxylic acid {1-[4-(4-benzyloxy-phenylamino)-piperidine-1-carbonyl]-3-methyl-butyl}-amide (Example 28) (0.30 g, 0.28 mmol) was dissolved in CH2Cl2 (5 mL) and treated with isovaleraldehyde (62 μL, 0.58 mmol). The reaction was stirred for 30 minutes at RT, then cooled to 0° C., treated with NaBH(OAc)3, allowed to warm to room temperature as the ice melted and stir overnight. The reaction was then diluted with EtOAc (100 mL), washed with saturated bicarbonate solution and brine, dried over Na2SO4, and concentrated. The residue was chromatographed on silica gel eluting with 3:2 hexane/EtOAc to give 0.28 g (82%) of the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06251918B1 |
| Source dataset | uspto-grants-2001_06 |
| ORD ID | ord-13702931ba96414d958bdf248cbc7b0f |
| Source note | uspto-grants-2001_06 |