HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbonic acid--N,N-diethylethanamine (1/2) → HCID 68817271, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbonic acid--N,N-diethylethanamine (1/2) | HCID 15264167 | — |
| Reactant | Trifluoroacetic acid methylene chloride | HCID 21863450 | — |
| Reactant | HCID 69185926 | HCID 69185926 | — |
| Product | HCID 68817271 | HCID 68817271 | — |
Reaction Steps
A solution of 1,1-dimethylethyl (2,3-dihydro[1,4]dioxino[2,3-c]pyridin-7-ylmethyl)(1-{2-[7-(methyloxy)-2-oxo-1,8-naphthyridin-1(2H)-yl]ethyl}-4-piperidinyl)carbamate (160 mg, 0.3 mmol) in TFA/dichloromethane (2 ml/2 ml) was allowed to stand at room temperature for 1 hour then evaporated to dryness, azeotroping with chloroform. The residue was dissolved in dichloromethane/methanol (10 ml/10 ml) and treated with MP-carbonate resin (2.5 mmol of carbonate per gramme, 4 g, 10 mmol). After 15 minutes the mixture was filtered, washing with dichloromethane then methanol (twice) followed by evaporation affording the free base of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071592B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-09d49428494b457290e5cc7d9526f2c4 |
| Source note | uspto-grants-2011_12 |