HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroformate → HCID 86663155, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | (S)-4-(2-chloro-6,7-dihydro-5H-pyrrolo[3,4-d]pyrimidin-4-yl)-3-methylmorpholine hydrochloride | HCID 86663150 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86663155 | HCID 86663155 | 112.3% |
Reaction Steps
(S)-4-(2-chloro-6,7-dihydro-5H-pyrrolo[3,4-d]pyrimidin-4-yl)-3-methylmorpholine hydrochloride (intermediate 6) (330 mg, 1.3 mmol), was dissolved in dry THF with srirring and treated with ethyl chloroformate (136 uL, 1.4 mmol) and NaHCO3 (218 mg, 2.6 mmol) at room temperature (20° C.) overnight. The mixture was concentrated in vacuo and the residue purified by flash chromatography using a mixture of 0-100% petrol ether/ethyl acetate as eluent, yielding the title compound (475 mg, 1.46 mmol, 41%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08785457B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-1a1589f3524742e4b53365bdfa546d2c |
| Source note | uspto-grants-2014_07 |