Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1-Propanol | HCID 1031 | — |
| Reactant | HCID 71698834 | HCID 71698834 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86700082 | HCID 86700082 | 82% |
Reaction Steps
1-Propanol (144 ml), water (96 ml) and concentrated hydrochloric acid (as 36%, d=1.18) (3.1 ml, 1.1 eq.) were added to the compound of Step 3 of Example 9 (20.00 g, 32.33 mmol) at room temperature. The mixture was warmed to 83° C. After confirming dissolution, the solution was cooled to 0° C. The seed crystals obtained above (20 mg) were then seeded, and the mixture was stirred for about 17 hours. The precipitated solid was then collected by filtration. The solid was then dried under reduced pressure at 40° C. overnight to give the title compound (18.26 g). Yield: 82%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08933103B2 |
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| Source dataset | uspto-grants-2015_01 |
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| ORD ID | ord-58f350e8f6cf49269cf52f44606b05b0 |
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| Source note | uspto-grants-2015_01 |
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