HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 14307792, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Benzene, 1-chloro-3-isocyanato- | HCID 17968 | — |
| Reactant | HCID 14654949 | HCID 14654949 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 14307792 | HCID 14307792 | — |
Reaction Steps
17α-Hydroxy-21-(1-piperazinyl)pregna-4,9(11)-diene-3,20-dione (EXAMPLE 6A, 5.00 g) is treated in DMF (20 ml) with m-chlorophenyliso-cyanate (1.84 g) for 3 days. The mixture is poured into water (200 ml). After 1 hr, the liquid is decanted. The solid is dissolved in methylene chloride and is extracted with aqueous sodium bicarbonate. The phases are separated and the organic phase is dried over sodium sulfate and concentrated. The concentrate is chromatographed on silica gel (3% methanol in methylene chloride to 4%) to give the title compound which is crystallized from hot ethyl acetate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05268477 |
| Source dataset | uspto-grants-1993_12 |
| ORD ID | ord-3988910fad94461e89c185e30c40ec99 |
| Source note | uspto-grants-1993_12 |