Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 90111597 | HCID 90111597 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 90112711 | HCID 90112711 | — |
Reaction Steps
tert-butyl N-[[(4R)-4-cyclopropyl-2,5-dioxo-imidazolidin-4-yl]methyl]carbamate (310 g, 1151 mmol) is dissolved in MeOH (3.1 L) at 6° C. 4M HCl in dioxane (310 mL) is added and the mixture warmed to 25° C. After stirring for 22 h, a second portion of 4M HCl in dioxane (110 mL) is added and stiffing continued for an additional 16 h. The reaction is then allowed to sit with no agitation for 2 days. The mixture is then diluted with toluene (6 L). The title compound is collected by filtration of the mixture as a white solid (180 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09206139B2 |
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| Source dataset | uspto-grants-2015_12 |
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| ORD ID | ord-410e78222e974309bba787e3767190a9 |
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| Source note | uspto-grants-2015_12 |
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