HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 21350203, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | (Diethylamino)sulfur trifluoride | HCID 123472 | — |
| Reactant | HCID 21350204 | HCID 21350204 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 21350203 | HCID 21350203 | — |
Reaction Steps
3 ml of dichloromethane was added to 0.18 ml of diethylaminosulfur trifluoride. Into the mixture was added dropwise a solution of 3 ml of dichloromethane containing 371 mg of 2-benzyl-3-methoxymethyloxy-6-[(3R)-3-hydroxy-2-pyrrolidinone-1-yl]pyridine under cooling in an ethanol/dry ice bath. The mixture was returned to room temperature and stirred for 2 hours. Then, water was added thereto, and the mixture was extracted with ethyl acetate. The organic phase was further washed with brine, dried over anhydrous sodium sulfate and the solvents was removed. The residue was subjected to silica gel column chromatography using 17-20% ethyl acetate/hexane as an eluent for separation and purification, to give 116 mg of the target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06599917B1 |
| Source dataset | uspto-grants-2003_07 |
| ORD ID | ord-3033169cdf7343f088df80a793e76baa |
| Source note | uspto-grants-2003_07 |