HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86642703, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Azepane | HCID 8119 | — |
| Reactant | 3-Azido-3-methylbutanoyl chloride | HCID 60134507 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 86642703 | HCID 86642703 | — |
Reaction Steps
To a stirred ice cold solution of 3-azido-3-methylbutanoyl chloride (8.00 g, 49.5 mmol) in anhydrous DCE (160 mL) was added azepane (12.6 mL, 3 equiv, 0.11 mol) in one portion. The reaction was stirred and left at 0° C. for 15 min and room temperature for 45 min. Aqueous 1 M HCl (100 mL) was added to the reaction mixture and the contents poured into a separatory funnel. The organic layer was separated and washed with 1 M HCl (100 mL) and saturated NaHCO3 (150 mL). It was dried over anhydrous MgSO4, filtered, concentrated and dried under high vacuum to give a crude oil (8.24 g, quant). This material was used without further purification. LRMS (ESI+) for C11H20N4O (224.1); Found: 225 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08278482B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-9846e14ca32b436d87c7fd6fdd5f78d0 |
| Source note | uspto-grants-2012_10 |