HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 21498935, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Phenacyl bromide | HCID 6259 | — |
| Reactant | 1-(3,6-Dihydro-2H-thiopyran-4-yl)pyrrolidine | HCID 13287468 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 21498935 | HCID 21498935 | — |
Reaction Steps
A solution of 56.3 g (0.28 mole) of phenacyl bromide in 100 ml. of dimethylformamide is added dropwise during 20 minutes under nitrogen to a cold stirred solution of 47.6 g (0.28 mole) of 5,6-dihydro-4-(1-pyrrolidinyl)-2H-thiopyran and 300 ml. of anhydrous dimethylformamide. After 2 hours, the solution is diluted with H2O and extracted with chloroform. The chloroform solution is washed with water, dried over magnesium sulfate and concentrated. The product is crystallized from ethanol to give crystals of 3-phenacyl-2,3,5,6-tetrahydrothiopyran-4-one. This is recrystallized from ethanol to yield crystals; m.p. 101.5° to 103.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03991076 |
| Source dataset | uspto-grants-1976_11 |
| ORD ID | ord-3a96b2aec49b4e048b9e045afcf22639 |
| Source note | uspto-grants-1976_11 |