HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 67369495, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 12801524 | HCID 12801524 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 67369495 | HCID 67369495 | 69.7% |
Reaction Steps
In an ice bath, 7.8 g of 15α-hydroxy-18-methyl-4-estren-17-one in 50 ml of pyridine is combined with 10 ml of methanesulfonic acid chloride. After 1 hour, 50 ml of dimethylformamide (DMF) is added thereto, along with 23 g of anhydrous sodium acetate. The mixture is stirred for another 20 hours at room temperature. The mixture is introduced into ice/water. The thus-precipitated product is vacuum-filtered, washed with water, dissolved in ethyl acetate, and dried. Crystallization from ethyl acetate yields 5.1 g of 18-methyl-4,15-estradien-17-one, mp 125.2° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04390530 |
| Source dataset | uspto-grants-1983_06 |
| ORD ID | ord-82f9264bb0e74aa383cd36657aa44139 |
| Source note | uspto-grants-1983_06 |