HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 6-[(6-Methylpyridin-2-yl)methyl]-1,4-oxazepane dihydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | tert-Butyl 6-[(6-methylpyridin-2-yl)methyl]-1,4-oxazepane-4-carboxylate | HCID 86630785 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | 6-[(6-Methylpyridin-2-yl)methyl]-1,4-oxazepane dihydrochloride | HCID 68536214 | 85.7% |
Reaction Steps
tert-Butyl 6-[(6-methylpyridin-2-yl)methyl]-1,4-oxazepane-4-carboxylate (Preparation 83, 42.5 g, 0.14 mol, 1 eq) was dissolved in isopropanol (250 mL), concentrated hydrogen chloride (38 mL, 0.42 mol, 3 eq) was added under stirring, and the mixture was refluxed for 2 h. The reaction mixture was then evaporated, and the residue was coevaporated twice with isopropanol. The product was crystallized from isopropanol, and the crystals were washed with diethylether/isopropanol (3:1) mixture and ether and finally vacuum-dried to give title compound as white crystals (32.3 g, 0.12 mol, 82%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08741934B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-13ca627fa0164ce2a5ad471ffb533998 |
| Source note | uspto-grants-2014_06 |