HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbonic acid, bis(1,1-dimethylethyl) ester → Tert-butyl (1-benzyl-4-hydroxy-4-piperidinyl)methylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbonic acid, bis(1,1-dimethylethyl) ester | HCID 10219638 | — |
| Reactant | 4-(Aminomethyl)-1-benzylpiperidin-4-ol | HCID 10421026 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | Tert-butyl (1-benzyl-4-hydroxy-4-piperidinyl)methylcarbamate | HCID 11759029 | 36.6% |
Reaction Steps
To a solution of 4-aminomethyl-1-benzyl-piperidin-4-ol (264 mmol, 58 g) in DCM (200 mL) and saturated NaHCO3 (200 mL) was added di-tert-butylcarbonate (396 mmol, 86.4 g). The reaction mixture was stirred for 12 hours. The layers were separated and the organic layer was washed with brine (50 mL) and evaporated. The product was purified on 1 L of SiO2 using a mixtures of ethyl acetate and DCM to give (1-benzyl-4-hydroxy-piperidin-4-ylmethyl)-carbamic acid tert-butyl ester (31 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09045461B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-b76c8aabfbc84270b7752213d311ad1c |
| Source note | uspto-grants-2015_06 |