HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 58474761, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3-Morpholinone | HCID 66953 | — |
| Reactant | HCID 58474527 | HCID 58474527 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58474761 | HCID 58474761 | 33.4% |
Reaction Steps
To a solution of 102 (350 mg, 0.842 mmol, scheme 26) in THF (10 mL) was added a solution of the anion [made from morpholin-3-one (340 mg, 4 eq., 3.37 mmol) and NaH (81 mg, 4 eq., 3.37 mmol)] in THF (5 mL)) and the mixture was heated to reflux for 8 hours. The mixture was quenched with saturated NH4Cl solution and extracted with DCM. The organic phase was collected, dried over anhydrous Na2SO4, filtered and concentrated. The resultant solid was triturated with acetone to give title compound 121 (135 mg, 33% yield) which was used in the next step with no additional purification. MS (m/z)=481.2 (M+H)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08906852B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-931cfadd6c184d27854ec83bce18be16 |
| Source note | uspto-grants-2014_12 |