HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → (6R)-6-(Hydroxymethyl)morpholin-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | 2-Chloro-N-[(2R)-2,3-dihydroxypropyl]acetamide | HCID 59613541 | — |
| Solvent | 2-Methyl-2-butanol | HCID 6405 | — |
| Product | (6R)-6-(Hydroxymethyl)morpholin-3-one | HCID 34179996 | 54.9% |
Reaction Steps
(R)-2-Chloro-N-(2,3-dihydroxypropyl)acetamide (1.31 g, 8.20 mmol) in tert-amyl alcohol (34 mL) was added dropwise over 2 h to a stirred solution of potassium tert-butoxide (2.30 g, 20.6 mmol) in tert-amyl alcohol (16 mL) at room temperature under nitrogen. After 1 hr, MeOH (8 mL) and water (0.5 mL) were added and the reaction mixture was stirred for an additional 20 min. The mixture was concentrated under vacuum and purified by flash column chromatography on silica gel, eluting with methanol/ethyl acetate (2/8) to give the title compound as a white solid (0.59 g, 54%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08367658B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-9d058689aeec4703b3abb3c41192bdb1 |
| Source note | uspto-grants-2013_02 |