HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 136057256, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 59644544 | HCID 59644544 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 136057256 | HCID 136057256 | 35.1% |
Reaction Steps
Add hydroxylamine hydrochloride (7 mg) to a 0° C. solution 5-[1-(3,5-bis-trifluoromethyl-benzyl)-5-phenyl-1H-[1,2,3]triazol-4-yl]-4-(2-chloro-benzyl)-4H-[1,2,4]triazole-3-carbaldehyde (50 mg) in 1,2-dichloroethane (1 mL). Stir 60 hours while allowing reaction to slowly warm to RT. Quench reaction by slowly adding 1 N NaOH (1 mL). Extract with CH2Cl2 (2×2 mL) and dry. Purification via silica gel chromatography using 3:1 to 1:1 hexanes:EtOAc gradient gives the desired product (18 mg, 35%). MS (IS) 606.1 (M+1); Rf=0.52 (1:1 hexanes:EtOAc).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07320994B2 |
| Source dataset | uspto-grants-2008_01 |
| ORD ID | ord-c44fb348b526438e99f948417aa17201 |
| Source note | uspto-grants-2008_01 |