HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Cyanide → HCID 22107240, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Cyanide | HCID 9032 | — |
| Reactant | HCID 19707529 | HCID 19707529 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22107240 | HCID 22107240 | 83.6% |
Reaction Steps
A mixture of 15.5 g (50.0 mmol) of 1,3-dihydroxy-xanthenium bisulfam [R. K. M. Pillai et al, J. Org. Chem. 51, 717 (1986)] and 4.90 g (75.0 mmol) of potassium cyanide in 150 ml of dimethylformamide is kept at 130° C. for 2 hours. The solvent is then concentrated on a vacuum rotary evaporator and the residue is taken up in ethyl acetate. The ethyl acetate phase is washed with water, dried over sodium sulfate and concentrated on a vacuum rotary evaporator. Chromatography of the residue over silica gel using the mobile phase system hexane/ethyl acetate=3:1 and crystallization of the pure fractions from ethyl acetate gives 10.0 g (83%) of 9-cyano-1,3-dihydroxy-xanthene, melting point 211°-215° C. (compound (107), Table 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05710198 |
| Source dataset | uspto-grants-1998_01 |
| ORD ID | ord-a8fb5d432a514bbd9d239da58858a39f |
| Source note | uspto-grants-1998_01 |