Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 4-tert-Butylpyridine | HCID 19878 | — |
| Product | HCID 12248299 | HCID 12248299 | 104.7% |
Reaction Steps
Add a solution of hydrogen chloride (4M in dioxane, 794.36 mmol, 198.59 mL) to 4-tert-butylpyridine (100 mL, 662 mmol) at 22° C. over 30 minutes. The internal temperature rises to 32° C.; control the exotherm with an ice-water bath and the by adjusting rate of the addition. Stir the mixture at 22° C. for one hour and concentrate. Wash the walls of the flask with EtOH. Dry the resulting solid under vacuum (1 mbar, 23-40° C.) to give the title compound as a white solid (119 g, 99%). MS (m/z): 136 (M-HCl+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09073856B2 |
|---|
| Source dataset | uspto-grants-2015_07 |
|---|
| ORD ID | ord-82d522197c6348e1aa34d8143bd5d96d |
|---|
| Source note | uspto-grants-2015_07 |
|---|