Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | 5-Oxo-4-(3-piperidin-1-yl-propyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester | HCID 66783496 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66783026 | HCID 66783026 | 97.2% |
Reaction Steps
A solution of 7.3 g (21.50 mmol) of 5-oxo-4-(3-piperidin-1-yl-propyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester was in 140 ml CH2Cl2, cooled to 0° C. and treated with 54 ml (215 mmol) of HCl solution (4 M dioxane), then warmed to RT. After 3 h, 40 ml of MeOH were added to dissolve the precipitation and stirring was continued over night. The solution was evaporated, dissolved in aq. sat. NaHCO3. solution, the water evaporated and the solid extracted with in CH2Cl2:MeOH 9:1. Concentration afforded the title compound 5.0 g (97%) as yellow oil. MS: 240.1 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08138175B2 |
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| Source dataset | uspto-grants-2012_03 |
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| ORD ID | ord-3ee64c0cb1ff41a1aab99d63ec7c51e4 |
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| Source note | uspto-grants-2012_03 |
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